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1-19#-LS-909-SIZE ANALYSIS MACHINE-user Manual PDF
1-19#-LS-909-SIZE ANALYSIS MACHINE-user Manual PDF
1-19#-LS-909-SIZE ANALYSIS MACHINE-user Manual PDF
Table of Contents
Chapter 1 Application, Principle of Measurement and Technical
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Assuming particles are uniformly and isotropically spherical, according to the Mie
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Scattering theory, the intensity of light scattering can be calculated upon the
Maxwell’s electromagnetic equation as
2
∞
2l + 1
Ia = ∑ {alπ l (cos θ ) + blτ l (cos θ )}
l =1 l ( l + 1)
2
∞
2l + 1
Ib = ∑ {blπ l (cos θ ) + alτ l (cos θ )}
l =1 l ( l + 1)
where
θ is the angle of scattering;
Ia is the scattered intensity of vertical polarized light of angle θ;
Ib is the scattered intensity of horizontal polarized light of angle θ;
where
1 4πσ c 2π
nˆ = (∈ +i ω= q= r
∈介 ω λ0 , λ介
), ;
∈介 is the dielectric constant of medium;
∈ is the dielectric constant of particles;
σ is the conductivity;
λ0 is the light wavelength in vacuum;
πq
ϕ l ( q) = J 1 ( q)
2 l+
2
ζ l (1) ( q) = ϕ l ( q) + iχ ( q)
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where
πq
χ l ( q) = − N 1 ( q)
2 l+
2 ;
J 1 ( q)
l+
2 is the Bessel function;
N 1 ( q)
l+
2 is the Neumann function;
l /2
( 2l − 2m )(l − 2m )
π l (cos θ ) = ∑ ( −1) m (cos θ ) l −2 m −1
m =0 2 m(l − m )(l − 2m )
l
1
= pl (cos θ )
(1)
sin θ
dπ l (cos θ ) d
τ l (cos θ ) = cos θπ l (cos θ ) − sin 2 θ = pl (cos θ )
(1)
d cos θ dθ
where
(1)
pl is the Associated Legendre Polynomial.
As it can strictly describe the scattered intensity of light, the Mie theory theoretically
applies for all kinds of particles. However, for large particles ( r 〉〉 λ ), its calculation is
very complex. Thus when calculating such large particles, diffraction formulas which
are simpler and more frequently used, will generally take the place. When particles
are infinitely far away from where they are observed, such diffraction formulas can be
simplified into the Fraunhoff equation as below:
A 2 2 J 1 ( kr sin θ )
2
I (θ ) = (πr 2)
(2
)
λf kr sin θ
Through observations, our R&D team has found that under the condition of r 〉〉 λ , the
Fraunhoff and Mie theories result in slight differences in displaying scattered light
intensities. However, in laser particle size analyzers, it is light energies (integral
between scattered light intensities and the receiving areas of detectors) that detectors
can directly receive and the receiving areas expand rapidly as receiving angles grows
on detector elements. We’ve discovered that around the angle of 14° (assuming that
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USER MANUAL OF LS-909
the refractive index of particles is 1.54, this angle accords with the scattered light
intensity of particles sized 1μm), the actual light energy is much larger than what is
predicted by the Fraunhoff theory. We therefore draw a conclusion that when the
receiving angle of a laser particle size analyzer is approximately equal or larger than
14°, in another word, when its lowest range is equal or smaller than 1μm, calculations
upon the Fraunhoff theory will result in obvious errors (an increase of the number of
particles sized around 1μm).
Assuming when there is no particle passing through the measurement window, the
light energy received by the central detector is E 0 and those by other detector elements
are E1 , E 2 ,L , E n in turn (due to aberration, dust scattering, etc.); when there are
particles in the window, the above light energies are represented
′ ′ ′ ′
by E 0 , E1 , E 2 ,L , E n , then
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′
E − E0
Obs = 0
E0
That is called obscuration. The higher in concentration the sample is dispersed, the
larger its obscuration will be.
′
S i = Ei − (1 − Obs )Ei (i = 1,2,L , n)
represents the scattered light intensity distribution, which also indicates the size
distribution of particles being analyzed.
By photoelectric detectors, the received light energies are converted into relevant
current signals, which are magnified and realize the A/D conversion on the
data-collecting card before being finally sent to the computer.
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above picture shows SCF-105B automated sample feeder and DPF-110 dry sample feeder,
As the core of the whole instrument, the mainframe realizes generation of the laser
beam, photoelectric conversion of scattered light energies, pre-processing and A/D
conversion of photoelectric signals.
The circulating sample feeding system is for transferring the samples to be tested into
the measuring unit, which shall be inserted into the mainframe of the instrument when
using, the dispersed samples are added into the sample feeding cell, and then the
circulating pump (wet-dispersion) /pressure-air (dry-dispersion) in sample feeder will
transfer the particles into the measuring window. The default configuration is
SCF-105B wet-dispersion automated sample feeding system for LS-909. We provide
several types of sample feeders for your choice. (The real configuration is subject to
your contract, the descriptions in the manual are only for reference.)
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USER MANUAL OF LS-909
The instrument needs to connect general-purpose computer for use, the computer
processes photoelectric signals, calculate the size distribution of samples upon the
detected energy distribution of scattered lights and organize the data into analysis
reports. The printer is responsible for outputting the hard copy of analysis reports, i.e.
printing.
The structure of the instrument mainframe of LS-909 is shown as Picture 2.2 (with the
cover removed).
Variety of sample feeding systems can be configured with LS-909, three types of
typical wet-dispersion sample feeders SCF-105B, SCF-126C, SCF-108 and one type
of dry-dispersion sample feeder-DPF-110 are shown as below. Insert the measurement
window into the measuring unit of mainframe, feed optimum dispersed samples to the
sample feeding cell and the circulation pump (or high pressure air) in sample feeder
will send the samples into the measurement window.
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SCF-105B is one type of automated circulating sample feeding system. Main parts use
316L stainless steel materials with good corrosion resistance, sample cell owns large
volume, high rotating speed and fast flow rate. SCF-105B can be configured with
several types of laser particle size analyzers.
SCF-105B is mainly used for those powders (water/alcohol as dispersion medium) or
emulsion. Please tell us if sample is magnetic or you need to use corrosive organic
solvent as dispersion medium, we will recommend you proper sample feeding system.
Parameters:
1. Power: 80W
2. Net weight: 10.3 kg
3. Dimensions: 210×260×345mm(L×W×H)
4. Motor speed: 400~4000rpm(stepless)
5. Built-in ultrasound, ultrasonic power 0~50W, stepless control
6. Suction height of self-priming pump: 0.8~1.5m。
7. Power adapter: input AC 220±10V 50Hz / output DC 24V/6.7A
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SCF-108 owns strong dispersion effect and strong suspension force for samples, it can
be attributed to turbopump and external propeller bicirculating drive system of sample
feeder as well as internal high-power ultrasonic probe. The circulating pipeline and
turbopump use stainless steel material, interior seal ring uses anti-corrosion silicone
rubber. The rotating speed of water pump and ultrasonic intensity can realizes stepless
adjustment. Configured with different windows, SCF-108 can match several kinds of
laser particle size analyzers to form a whole set of particle size measurement system.
Parameters:
1. Power: 100W
2. Net weight:12kg
3. Volume of sample cell (measurement window and pipeline excluded): 500/1000ml
4. Dimensions: 265×325×405mm (L×W×H)
5. Pump speed: 600~4000 rpm (stepless)
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This chapter specifies the requirements on the basic and affiliated equipment for the
installation of the instrument, as well as those on the working conditions, which have
been derived from the instrument’s technical characteristics and our experience in
service through years. Following the instructions can not only avoid as many
problems in operation as possible, but prolong the lifespan of the instrument so as to
improve effects in use.
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USER MANUAL OF LS-909
Working Environment
Power Supply
Warning:
(a) In case of unstable power supply or instant disturbances, for example, frequent
powers on and off of a nearby high voltage electrical equipment, a purified
regulated power supply ≥1000W for the measuring unit is required;
(b) The ground wire of the instrument should not be connected with other ground
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wires.
Working Table
The working table should be rigidly placed on the ground, a table with the
length≥1.5m, width ≥0.75m and the height around 75cm will be fine. More than 100
kgs of pressure can be sustained by the table-board and no deformation resulted. The
computer and the printer should have separate tables.
Computer
A computer with the good running of Windows XP or Windows 7 (32-bit version) is
required, it also should be equipped with a nine-pin R232 serial port (individual
printer models may have compatibility issues).
Printer
Printers that are generally compatible with PC (individual printer models may have
compatibility issues).
Air Conditioner
The operating area should be in a temperature of 10-30℃ and a humidity below 85%,
otherwise an air conditioner with enough power (based on the area of the operating
place) and a function of humidity removal is required.
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USER MANUAL OF LS-909
If the laboratory temperature is low (<10oC) and the humidity is high (>90%), when
the measurement window of sample cell is inserted in the measuring unit, mist will
occur on the glass gradually because the temperature on the surface of the glass is
obviously lower than the temperature inside the measuring unit. The mist will scatter
light and affect the measuring results.
The mist won’t occur immediately when the measurement window is inserted into the
measuring unit. It occurs slowly and disappears automatically. Thus, the background
light energy becomes higher gradually and returns to normal little by little. If the
background light energy is much higher than usual, pull out the measurement window,
you’ll see a layer of mist on the glass.
Obviously, the background and sample measurement can’t be performed when the
mist exits, the mist will disappear automatically, and the mist on the Static Sample
Feeder disappears faster than that on the Sample Circulation Feeder.
4.1 Unpacking
A highly precise instrument with optical, mechanical and electronic integration,
LS-POP (9) requires handling with care in conveyance. Please follow the steps below
when unpacking the instrument.
1. Check the followings before unpacking:
(a) Is the package placed upside down?
(b) Is there any damage on the package?
(c) Is there any hint of being watered on the package?
2. It is required that unpacking should be instructed by our technicians. Uninstructed
unpacking should be approved by our company;
3. Avoid crashes of the instrument during unpacking and never drop. Handle with
care when taking the parts out of the package. Save the fillings and the packing
box in case of future conveyances;
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USER MANUAL OF LS-909
4. Please do not throw pearl wool, dustproof bag away after unpacking but handle
them after checking of all materials so as to avoid the loss of some small gadgets
which are put in inconspicuous place.
5. Check the packed items with the packing list. For any unconformity, please
contact our after-sale service department as soon as possible.
System
1. There are 4 fixed pipe joints for SCF-105B, including 2 joints of sample circulating
pipe on the left, 1 for water inlet pipe and 1 for drainage pipe on the right. Connect the
circulating pipe joints with the measurement window, you can check if your
connection is correct by observing if the water flowing from bottom to top. The pipe
diameter of drainage is bigger than that of inlet which is used to connect to the water
source. This equipment owns water suction pump, the stress-free water container or
stressful water supply pipe can be used as water source. SCF-105B is full-automatic,
without operating button, all the actions will be controlled by software automatically.
2. Find the measurement window in the accessories box and remove the dustproof
casing. Blow off the dust with the ear syringe ball and do some cleaning if necessary.
Fasten the other end of each of the two pipes (in the circulating pipe joints) which
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USER MANUAL OF LS-909
have been fixed on the inlet and the outlet of the sample feeder to the 2 pipe joints in
the measurement window; Tube connection relies on the elasticity of rubber tube for
connecting and sealing, please make sure the reliability of connection.
3. Power interface, control signal line port and power switch are in the back of
SCF-105B, it’s easy to distinguish the ports by shapes.
1. Find the measurement window in the accessories box and remove the
dustproof casing. Blow off the dust with rubber suction bulb and do some
cleaning if necessary. Fasten the inlet and the outlet pipelines of the sample
feeder to the measurement window, the inlet pipe joint connects the upper pipe
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USER MANUAL OF LS-909
of the measurement window and the outlet pipe joint connects the lower one
(the connection way must be correct). The wastewater discharge outlet is in
the back of instrument, connect it with discharge pipe and put the wastewater
discharge pipe in the liquid waste recovery container, the liquid waste is
discharged by flowing automatically without pressure so the liquid level of
liquid waste container should be lower than the base of sample feeder. Insert
the measurement window into the middle slot of instrument mainframe.
2. Insert the special direct-current power supply plug into the socket in the back
of sample feeder, turn on the power switch, the power indicator lights up.
3. Add the circulatory medium (100~150ml) into the circulating sample cell by
using the measuring glass, different window pipeline will result in different
capacity. Too few mediums will cause plenty of bubbles after circulation, keep
the liquid level at least a 10mm distance from the mouth of cell after adding
the samples.
Attention: When you don’t use the instrument please close the water pump
of sample feeder (adjust pump speed to stop state.) Idling of water pump for
long time will lead the damage of water pump.
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USER MANUAL OF LS-909
1. Find the measurement window in the accessories box and remove the
dustproof casing. Blow off the dust with the rubber suction bulb and do some
cleaning if necessary. Insert the measurement window to the mainframe, take
out 2 rubber pipes from the accessories box and fasten one end of each of them
into 2 pipe joints of the measurement window to the end. The upper joint
connects the inlet mouthpiece (marked in blue rubber ring) of the sample
feeder and the below joint connects the outlet mouthpiece (marked in red
rubber ring). The connections must be correct.
2. Take out the plastic coaster from the accessories box and insert it along the
bottom of the front of the sample feeding system into the card slot. Take out
the measuring cup from the accessories box and clean it up, pour moderate
clear water into it, lift the upper shield of SCF-108 up, put the measuring cup
onto the groove of the plastic coaster and put down the shield.
3. Take out the power supply and power line from the accessories box, insert the
end of power output into the slot of power supply in the back of SCF-108,
connect the input end with the power line which is plugged in 220V
multi-purpose socket.
4. Turn on the power of SCF-108, the power indicator in the control panel lights
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USER MANUAL OF LS-909
up. Switch on the circulating pump by control panel and adjust the rotating
speed to 2500 rpm. Observe if there is water leaking in the measurement
window, if leakage occurred, please use the tool in the accessories box to
screw the junk ring on the window moderately until the leakage stops.
5. Stop the circulation by the control panel, lift up the upper shield of SCF-108
and pour away the water in the cup, switch off the power supply. The
installation of SCF-108 is finished.
1. Find the measurement window in the accessories box and remove the
dustproof casing. Blow off the dust with the rubber suction bulb and do some
cleaning if necessary. Insert the measurement window into the mainframe, put
the air compressor and dust collector in right place, please turn on the power
switch in the dust collector, connect the pipe of dust collector to the dust
collection exit of measurement window, power line inserted into the control
box configured.
Attention:
The actions of dust collector are controlled by the control box
automatically, so this step must be correct.
2. Take out the transparent high-pressure air pipe from accessories box, cut out
few segments according to the distance between instrument and air
compressor (the pipes shall be kept as short as possible in the premise of
successful connections so as to reduce the pressure loss in the airflow).
3. Use high-pressure air pipe to connect air compressor, oil-water filter and
sample feeder (refer to Picture 4.8 as below), connect one end of feeding pipe
to sample outlet connection of sample feeder, the other end to sample feeding
connector of measurement window, connect negative pressure detecting tube
respectively to the negative pressure detecting ports of instrument mainframe
and sample feeder.. The feeding pipe is thicker than high-pressure air tube, the
diameter of negative pressure detecting tube is the same with high-pressure air
tube’s but the former’s material is slightly softer, high-pressure air pipe joints
are special quick-change connectors, the interior pressures of negative
pressure detecting tube and feeding pipe are small, can be directly inserted into
the pipe joints relying on their own elasticity.
4. Take out the special power lines of sample feeder and instrument mainframe
from the accessories box, insert the ends of power output into the slot of power
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USER MANUAL OF LS-909
supply in the back of instrument and sample feeder, connect the input ends
with the power line which is plugged in 220V multi-purpose socket. Connect
the signal line with sample feeder, instrument mainframe, control box and
computer, the ports of signal line are universal you only need to notice the
shapes of ports.
5. After confirming the connection is ok, turn on the power switch of air
compressor, the air compressor will stop automatically when the pressure set
in advance is reached, no need to operate artificially. Check if the connection
of gas circuit is ok, if any air leakage, if normal, the connections of DPF-110
are finished.
Attention: Please cover the original dust cover on measurement window when
you pull out the window or you don’t use the instrument, to avoid dust from
entering the instrument inside.
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Sample Feeder
Unit Connections
1. If the manual sample feeder is configured, you only need to connect the signal line
of instrument to the USB interface of computer.
2. If the automated sample feeders are configured (SCF-105B, DPF-110),
Insert one end of the signal wire (RS-232 nine-pin serial port line) which is enclosed
in the accessories box into the communication interface of the instrument mainframe
and the other end into serial line interface of the sample feeder (omit this step for
manual sample feeder). DPF-110 has two universal interfaces of signal line, two
signal lines are equipped, these two signal lines, one is for connecting instrument
mainframe and sample feeder and another is for connecting sample feeder and the
control box of dust collector.)
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Remark: There will be a reminder of registration software when you run it for
the first time, a temporary registration code which is saved in a file named
“sn.txt” can be found in CD, a permanent code will be given by omec after full
payments for the instrument being paid off. The interface of installation and
software registration will be a little different for different versions of software.
Any questions please call: +86 756 3395365.
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Operating steps:
1. Switch on the mainframe of instrument (preheating for 30 minutes) and sample
feeder.
computer desktop, enter the main interface of the software (as below):
If “The measuring instrument has been found” appears on the lower left corner of
the interface, it means the instrument and the computer have been connected.
The upper left yellow part is background optional energy signal window, a very
important information window for observing the working status of the instrument.
The detector numbers are shown in the horizontal axis, “0” (also called as “column 0”)
is located in 0°angle of the optical axis of instrument, the angles of the subsequent
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detectors diverging from the optical axis increase successively. The left red column
represents for the laser intensity of “column 0”, the blue column represents for the
light energy signal which can be received by the corresponding detectors, the stronger
the signal is, the higher the column will be. After adding water into the sample feeder
for circulation, in normal standby mode, column 0 will be above 70%, column 1 will
not exceed 50 and other columns will decrease successively, the fluctuations of
background become smaller as time goes by. If the signals don’t show like this, this
could be due to the centering alignment of light path hasn’t been done (alignment is to
align the laser beam to No. 0 detector). The user can finish the alignment by clicking
“system alignment” in the toolbar.
The circulating pump of the sample feeder is not suitable for long-time work, so
please temporarily close it after confirming the status of instrument and start it again
when you begin the measurement.
The instrument can be configured with different types of sample feeders for manual
measurement, the following is an example of SCF-108 sample feeder’s measuring
procedures:
1. Create a new measuring file: click “new” icon under “start” tab of the software,
follow the prompts to create a new measuring file for the save of measuring records.
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1. Set up the measuring parameters: refer to picture below, switch the menu bar
to “measure” tab, select correct refractive index of sample material
interval .
2. Turn on circulating sample feeder: add water into the sample cell, adjust to
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high rotating speed circulating for 10 seconds and stop 5-10 seconds, repeat
this step for several times until the air bubbles eliminated completely, and then
adjust the rotating speed of circulation to that you need. (if SCF-105B
configured, follow up the steps: “tool->sample feeder->add water-> exhaust
air bubbles-> set up pump speed” )
3. System alignment: If the background state is unsatisfactory, click “system
alignment” button under “tool” option, click “auto” button on the pop-up panel.
You can also input suitable stepping, click “up, down, left, right” button for
manual adjustment; if the background is fine, directly go to the next step.
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The main functions of measurement prompt area and sample feeder status’ display
area: give the user some prompts during the measurement of samples and display the
current status of automatic sample feeder.
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7. Cleaning of sample feeder: after the measurement is finished, drain the waste
water in the sample cell and pour cleaning water into it for circulation,
generally repeat the steps for 3 times. (Observing the background, the cleaning
times depends on the background status.)
The instrument can use SOP for automated measurement, the following is an example
of SCF-105B sample feeder’s measuring procedures:
1. Confirm if the instrument mainframe and sample feeder have been connected
before running SOP, the connection status show as below picture:
2. Create a new measuring file: click “new” icon under “start” tab of the software,
follow the prompts to create a new measuring file for the save of measuring
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records.
3. If SOP hasn’t been created, please refer to subsequent chapter “new SOP file” to
create it (SOP-standard operating procedure), this file can be edited if necessary.
4. Click “run SOP…" under “measure” options, a dialogbox pops up as below:
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5. Choose the newly-created SOP, click “ok” button the instrument runs
according to the settings of SOP, the system will measure “electric
background” and “light background” automatically, and then get into the state
of waiting for samples adding as picture below, you can pour the samples into
the sampling cell of the sample feeder.
As samples’ adding, it can be observed that the scattering light energy signals
appear and beam obscuration column rises gradually. The column of beam
obscuration is green if it’s in normal range, otherwise, it’s red. Pay attention to
the change of beam obscuration which shall be controlled within the upper and
lower limit (can be set up, for example: 5%-15%), the color is green. Beam
obscuration indicates the concentration of samples, the requirements for the
sample concentration is different as the different samples.
6. When beam obscuration is in normal range, click “measure sample” under
“measurement” options, wait for a moment, you can see the measuring record in
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the record list on the right side of the software, we set up the default sampling
frequency as 3, so 3 measuring records will be generated.
7. After the measurement is finished, the measuring software will clean the sample
feeder automatically if the auto cleaning function has been selected in SOP. So far,
SOP measurement is finished as picture below.
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fitting report
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statistical report
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Steps:
1. Switch on the mainframe of instrument (preheating for 5-15 minutes) and sample
feeder, open dryer and air compressor.
If “The measuring instrument has been found” appears on the lower left corner of the
interface, it means the instrument and the computer have been connected. If the
instrument isn’t connected well SOP cannot run. We choose DPF-110 dry-dispersion
sample feeder as an example in this user manual.
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1.Create a new measuring file: click “new” icon under “start” tab of the software,
follow the prompts to create a new measuring file for the save of measuring
records.
2.Set up the measuring parameters: switch the menu bar to “measure” tab, select
correct sample material (silicon carbide 2.6 0.1), select proper one-time sampling
time (10-15 seconds), background measuring time (10-15 seconds), analysis mode
(3 modes: general mode, general enhanced mode, unimodal mode, we usually
choose general model). Input sample name (silicon carbide), sample no.(1200#),
sampling frequency (3) and sampling interval (0.0 second), create average results
and so on. Click “more parameters” in the right of menu bar to set up advanced
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parameters (usually you don’t have to revise it), shape factor (6), analysis scope
(0.02-2100), if enable the reminder for beam obscuration (suggest to choose yes),
the upper and lower limit value of beam obscuration (1%-10%). Click “dispersion
pressure” to set up it (0-600 kpa) and fluctuating value of dispersion pressure
(0-100%).
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4.Sample adding: adjust the mouth size of hopper, add samples into it.
5.Measure background:Enter airflow pattern: click “sample feeder” under “tool” tab
control, click “airflow” in pop-up control panel.
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Adjust to proper dispersion pressure by adjusting knob of sample feeder (display area
of sample feeder status will show the current dispersion pressure), negative pressure
is required to be above 1000pa, if not the instrument cannot work.
The main functions of measurement prompt area and sample feeder status’ display
area: give the user some prompts during the measurement of samples and display
the current status of automatic sample feeder (as below).
If the current background is in good condition, click “start” button under “measure”
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6.Sample measurement: click “sample feeding” in the control panel of sample feeder,
adjust the speed of sample feeding, click “measure sample” button under
“measurement” option when the beam obscuration is in proper range.
7. Measurement result: after measurement is finished, you can see the measuring
records in the measuring record list on the right side of the software
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Before measurement, confirm the instrument and sample feeder have been connected.
The default is automated alignment when you run SOP in the first time.
1.Create a new measuring file: click “new” icon under “start” tab of the software,
follow the prompts to create a new measuring file for the save of measuring
records.
2.Sample adding: Adjust the mouth size of hopper, add samples into it.
3.Click “run SOP…" under “measure” options, a dialogbox pops up as below:
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If SOP hasn’t been created, please refer to subsequent chapter “new SOP file” to
create it (SOP-standard operating procedure), this file can be edited if necessary.
4.Choose the newly-created SOP, click “ok” button the instrument runs according to
the settings of SOP, the system will measure “electric background” and “light
background” automatically, and then get into the state of waiting for samples
adding as picture below, When beam obscuration is in appropriate range, click
“measure” button, the system will start the measurement automatically.
Please refer to the picture below for appropriate value of beam obscuration.
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5. Wait for a moment, you can see the measuring records in the measuring record
list on the right side of the software, we set up the sampling frequency as 3, so
3 measuring records generate.
After the measurement is finished, the measuring software will clean the sample
feeder automatically if the auto cleaning function has been selected in SOP. So far,
SOP measurement is finished.
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Open “sample material”, if the parameter you need appears in the drop-down box, you
can select the parameter directly and click “ok”, the software will reanalyze the report
and generate a new report. If no parameter needed, click “more” under sample
material, a dialog box appears as below:
The user can move the items of sample material you need to “frequently-used sample
materials” on the right from “not frequently-used sample materials” on the left, and
click “ok”, the software will reanalyze the report and generate a new report.
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The user can fill in “sample material”, “refractive index”, “absorptivity” and “density”
according to the actual situation, and click “insert”, the parameters edited will be
recorded in the sample material database and will show in the list of “commonly-used
sample materials”.
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2.Sample material
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Sample material: a major parameter, if the user cannot find the material needed in the
current sample material listing, please click “sample material…..” button to add,
delete or revise it (refer to the previous chapter).
Dispersion medium: if the user cannot find the material needed in the current
dispersion medium listing, please click “dispersion medium…..” button to add, delete
or revise it (refer to previous chapter).
Analysis mode’s selection: general mode, enhanced mode, unimodal mode, you can
choose general mode if you don’t know the distribution of the samples.
Shape factor: is used for calculating specific surface area, please set up the value as
the default 6 (the shape factor of spheriform is 6) if you are not interested in it, if you
want to obtain the accurate specific surface area you need to input the shape factor of
the sample being measured.
3. Identification: sample name, sample number, remark. The above parameters you
set up will show in the measuring report.
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Different sample feeders will have differences in setup (for example: SCF-105B).
Rotating speed of water pump (0-4000)
Ultrasonic mode (if choose ultrasonic, timing ultrasound before measurement,
continuous ultrasound during measurement, continuous ultrasound after electrical
background
Ultrasonic power (0%-100%)
Ultrasonic time (only available when timing ultrasound before measurement is
selected as ultrasonic mode)
Cooling time (only available when timing ultrasound before measurement is selected
as ultrasonic mode)
Time interval (only available when continuous ultrasound after electrical background
is selected as ultrasonic mode)
6.Sampling circulation
Different sample feeders will have differences in setup (for example: SCF-105B).
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Numbers of round for sampling (numbers of each round for repeated sampling)
Sampling frequency per round (times of sampling each round)
Sampling interval (stop how many seconds between each time’s sampling)
Create average result (if checked, the average result will be added after each
measurement automatically)
Cleaning mode (cleaning before measurement, cleaning after measurement)
Times of repetition (default is 2)
Bubbles exhausting (when bubbles exist in the dispersion medium in the sampling cell,
check “bubbles exhausting” to discharge the bubbles, so as to keep the background
measured from the impact of bubbles)
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User particle diameter…: only available for the records generated in this SOP
measurement, user particle diameter under “start” menu bar in the main
interface is only available for the records generated in manual measurement.
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1.Sample feeder
Choose the proper sample feeder, dry dispersion chooses DPF-110.
2.Sample material
Sample material: choose proper sample material
Dispersion medium: you don’t need to choose it because the medium of dry
dispersion is air, so if you choose dry-dispersion sample feeder, this parameter is
hidden.
Analysis mode’s selection: general mode, enhanced mode, unimodal mode, you can
choose general mode if you don’t know the distribution of the samples.
Shape factor: is used for calculating specific surface area, please set up the value as
the default 6 (the shape factor of spheriform is 6) if you are not interested in it, if you
want to obtain the accurate specific surface area you need to input the shape factor of
the sample being measured.
Setup of beam obscuration range: you will be prompted during the measurement after
setting up this range (generally 1%-10%).
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USER MANUAL OF LS-909
Filter the data beyond the range of beam obscuration: after this button is checked the
software will filter the data beyond the range of beam obscuration in the measurement
automatically.
Timeout: the software will stop sampling in any case after the time you set up reaches
and will give you a prompt.
3.Identification: sample name, sample number, remark. The above parameters you set
up will show in the measuring report.
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5. Setup of sample feeder: (the parameters will be different for different sample
feeder)
Speed rate of sample feeding: can set 0%-100%, usually we set as 60%-90%.
Cleaning: operate the cleaning after measurement is finished.
Setup of dispersion pressure’s fluctuating value: monitor the dispersion pressure in the
process of measurement, to keep the pressure in a constant range during the sampling
procedure. There will be a prompt in the record if this range is exceeded.
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User particle diameter…: only available for the records generated in this SOP
measurement, user particle diameter under “start” menu bar in the main interface is
only available for the records generated in manual measurement.
After finishing the setup of above options, click “ok”, a dialog box will pop up,
choose proper path and input file name, click “save”, you finish the new SOP file.
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Different users focus on different size distribution data, the default data format cannot
meet all users’ requirements so our software adds the settings of size grading which
enables the user to set up the size grading value in the size distribution table of the
measuring report by themselves so as to realize the free choice of the concerns of
grain size. Besides SOP advance setup in Chapter 7.2.7 and “manual measurement” in
start menu, you can also set up it through editing measurement records after the
measurement is finished.
Check one measurement record, right-click to select “edit”- “identify”- “user size”, a
dialog box of editing user size will pop up.
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Remark: click user size under “start” menu bar in the main interface, the
dialogbox shows the particle diameter set by the user last time (if the particle
diameter hasn’t been revised by the user, the value is default). The default of
user’s particle diameter by SOP shows when SOP is created, the particle
diameter saved shows when SOP is edited.
Click the item you need to edit listed in the size grading listing in the right side of the
dialogbox (selected item will show in dark color), input the needed value in the left
textbox of the dialogbox, click “revise” button, click “ok” after the setup is finished.
What needs your attention is, the value revised must submit to the order rule of
arranging from small to large for the values in the size grading listing, if you want to
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USER MANUAL OF LS-909
revise the value “0.160”, to ensure the value revised larger than the last item’s value
and smaller than the next item’s value.
Generate:
Lower limit of particle size: 0.02μm
Upper limit of particle size: 2100μm
Particle size grading value: maximum (100), minimum (2)
Linear: generate the linear particle size
Logarithm: generate the logarithm particle size
Update: click this button, the particle size will be generated.
The measuring software can be exported as excel file, the precondition is Microsoft
office software and relevant excel components have been installed. Open a measuring
report, click “file menu”- “data export”, a dialogbox will pop up as below, input a file
name, click “ok” to save it.
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Thorough reading on this chapter and necessary practices as required will help users
in standard operations on the instrument.
1. Particle Diameter
Also called particle size, it symbolizes how big or small a particle is. Except for that
of spherical particles, particle diameter is an equivalent size which changes according
to different working theories of instruments, rather than a real physical size. In the
theory of light scattering which applies in particle size measurement, particle diameter
is considered as the diameter (distribution) of spherical particle (s) which has (have)
the same optical property and the most similar performance in light scattering as the
particles to be analyzed.
3. Distribution Mode
It’s the rule by which the sampled particles are distributed in size. There are four
models available in LS-POP (9): General, Enhanced, Rosin-Ram and Single. General
is suitable for common samples, Enhanced mode is for wide –distribution samples,
Rosin-Ram (R-R), which is preferable for single-crest size distribution, and Single
mode is more applicable for monodisperse samples.
5. Obscuration
Percentage or fraction of the illuminating light that is attenuated due to extinction
(scattering and/or absorption) by the particles. A large obscuration indicates a high
concentration of the sample.
Appropriate suspension mediums refer to those liquids 1) which can neither cause
chemical changes on the sample nor dissolve the sample; 2) which can make the
sample fully soak in it and will not corrode the pipeline; 3) which are easy to clean up
after use; 4) which are economical. Condition 1) and 2) are required while Condition
3) and 4) are not necessary but helpful. Water is the most commonly used suspension
medium.
Dispersants are those chemicals which are used to optimize the dispersion of sample
in the suspension medium and reduce agglomerations among particles. Sodium
hexametaphosphate is one of those dispersants which are easily found in market. The
volume of dispersant for a certain sample can be decided upon users’ experience.
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Auxiliary dispersion devices have stirrer and ultrasonic oscillator. If the sample is fine
and is easy to converge, these devices can help to disperse the agglomerates by
external force. The handling time of the sample in the device depends on the
circumstances, generally it will be between dozens of seconds and ten minutes.
The following is the flow chart of sample preparation for your reference:
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Results
In the measurement, many factors will distort the result, for example, insufficient
sample dispersing, air bubble in suspension liquid, dew on the measurement window,
sedimentation of big particles, unrepresentative sampling, and so on. This section
introduces the methods to judge the authenticity of measurement results, the reasons
for distortion and its solutions.
measurement results
Repeatability (reproducibility) is the result variations for the same sample analyzed by
the same instrument. The repeatability is represented with three analyzing value, they
are average diameter (volume average diameter, or D50), upper limit diameter (D90,
D95), lower limit diameter (D10, D7). For the repeatability of D50, its repeatability
error shall be controlled within 5% in the measurement of homogeneous samples. For
boundary diameter(D90、D10), its repeatability error shall be controlled within 10%.
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For this analyzer, repeatability is defined with the relative standard deviation of the
characteristic particle diameters of the particles being measured.
The quadratic mean deviation and relative deviation of analyzing value can be
calculated automatically by the statistic report in software of this analyzer.
microscope. If there are two or more particles adhere to each other in the liquid, it
indicates the sample is not well dispersed. Sometimes the repeatability of measuring
results can also reflect the dispersing condition. Review the repeatability of measuring
results of multiple sampling, the measuring results of samples not well dispersed is
always unstable.
Since liquid is used in measuring, air bubbles are easily generated. The bubbles also
scatter the light as the particles do, which disturbs the measurement.
Causes of air bubbles:
(1)The bubbles were not eliminated completely before closing the cover of Static
Sample Feeder;
(2)The air in the circulating system is not exhausted;
(3)The circulating speed is too high;
(4) The dispersant contains vesicant;
(5)The suspension is made of two liquids(e.g. ethanol and water);
In situation (1), bubbles can be seen in the widow of Static Sample Feeder with eyes.
Here we mainly discuss the bubbles caused by other reasons, they are in the Sample
Circulation Feeder.
In situation (2), bubbles are big and can be observed from the measurement window
of sample circulation feeder. They can also be inferred by the background light energy
distribution, if bubbles exists, the background light energy is stronger than normal and
isn’t stable. The bubbles will disappear after circulating for a while.
In situation (3), bubbles can also be seen from the measurement window. From
background light distribution we can see the speed of circulating obviously influence
the bubbles. If there are bubbles with high circulating speed, lower the speed.
The dispersant containing vesicant can only be used in Static Sample Feeder, if it is
used in Sample Circulation Feeder, a large number of bubbles will be generated.
When suspension liquid and vesicant are mixed but without churning up, bubbles
wouldn’t occur. After the Sample Circulation Feeder starts circulating, bubbles will
increase gradually. The symptoms of bubbles generated in situation (5) and (4) are
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similar. When the condition is serious, the transparent suspension liquid will turn into
white and the background light energy will increase obviously.
To observe small quantity of bubbles in these two situations, please follow the below
steps:
Step 1: set the circulating speed to the lowest, the instrument in background
measurement status;
Step 2: start circulating, after it works correctly (around 3 minutes later), perform
background sampling;
Step 3: after the background sampling is finished (the background measurement
button on the screen changes into sample analyzing), adjust the circulating speed to a
higher level (there couldn’t be burble in sample trough), watch the light distribution
(in fact no sample exists).
If the light distribution is stable and smooth, it indicates that the bubbles exists, the
light energy you see is from the bubbles scattering.
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Analyzing the sample with Sample Circulation Feeder, all particles of the sample in
trough should have the same chance to join the circulation for assuring the
representative measurement. But in actual analyzing, big particles (for example, the
particles with diameters >200μm or particles with density > 4g/cm3) easily sink in
pipelines, so that they couldn’t be measured which will result in a smaller analyzing
result. Therefore, we should avoid the sinking of big particles during sample
analyzing.
There are several approaches to avoid or decrease the sedimentation of big particles.
1) Improve the circulating speed under the precondition of avoiding generating
bubbles.
2) Choose a suspension liquid with higher viscosity.
3) If sedimentation can’t be avoided, shorten the interval between sample input and
data collection.
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Except for regular cleaning, complete cleaning of the measurement window is also
required when the window gets dirty or fails in keeping the transparency.
Before each day’s first analysis, check the measurement window to make sure if there
is any need for cleaning. The window glasses getting dirty, declining in transparency
or being seriously rubbed on surface will result in the rising of the Background light
energies and thus cause a narrowed width of particle size distribution.
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Three factors may do harm to health through operation, i.e., laser radiation, electricity
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and hazardous samples. Special attention should be paid under the following
instructions.
Laser radiation
He-Ne laser source is applied in the instrument with an output power of 2mW and
generates red laser beam with a wavelength of 0.6328μm.
WARNING
Looking into the direct path of the laser beam can cause permanent eye damage.
Directly looking into the laser beam or its reflection (on mirrors or polished metal
surfaces) can cause eye damage. Safe use is available only when people who operate,
maintain and repair the instrument have a basic knowledge of high intensity and
coherence of the laser beam.
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personnel.
4. When using dry-dispersion sample feeding system for sample measurement,
please confirm if the powders to be measured are suitable for being dispersed in high
pressure air. For those flammable, explosive and poisonous powders, please consider
the safety problem of dust explosion prevention. This dust collection system is
common for civil use, poisonous dust as object isn’t taken into consideration.
Namely, particle diameter is the diameter of a particle, which describes the size of the
particle. In the case of a spherical particle (see Picture A-1(b)), particle diameter
equals the diameter of the sphere.
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However, on more conditions, the shapes of particles are neither regular nor spherical
(see Picture A-1(a)). Description of the size of such particles, as a matter of fact, relies
on many a parameter. Yet in practice, the usual condition in which a sample is made
up of numerous particles which vary in size and shape, allows only one parameter, i.e.
particle diameter, to describe the sizes of particles. This particle diameter is usually an
equivalent value under a certain method and condition of measuring, rather than a real
physical size of the particle to be analyzed.
xi = xi −1 xi , i = 1,2,......, m.
How to choose the above methods of size distribution in practice relies on different
needs and customs.
On most conditions, we only care about the relative values concerning particles
(number, weight or surface area). Therefore, such particle size distributions are
usually normalized as ni / N , wi / W and si / S , to respectively symbolize the number,
weight and surface area distributions of particle size, where
m m m
i = 1,2,..., m; N = ∑ ni ,W = ∑ wi , S = ∑ si
i −1 i =1 i =1
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∑ ni , = ∑ wi , = ∑ si = 1
i =1 i =1 i =1
Where
i = 1,2,......., m; Yi , the accumulative distribution, symbolizes the percentage of the
to describe the percentage of the particles whose diameters are above xi to all
particles to be analyzed. Apparently
Yi + Yi `= 1
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Though particle size distribution can provide a relatively overall and detailed
description of the sizes of the analyzed particles, it is not available for an instant
knowledge due to the abundant data it displays. Therefore, those diameters, which can
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symbolize some characteristics of the sampled particles, are used for simplification.
Such diameters are called characteristic diameters.
Mean Diameter
In the following equation:
m m
x( p, q ) = (∑ ni xi ) /(∑ ni xi )
p q
i =1 i =1
xi = ( xi −1 xi),which is the mean diameter of particles whose diameter are within the
range of Interval i.
i =1 i =1
3
As ni xi is proportional to the total volume (weight) of all the particles within the
range of Interval i, x(4,3) means the weighted average of particle diameter to volume
(weight), which is called volume or weight mean diameter.
The above equation shows the weighted average of particle diameter to the amount of
particles, which is called particle amount mean diameter.
i =1 i =1
2
As ni xi is proportional to the total surface area of all the particles within the range
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of Interval i, x(3,2) means the weighted average of particle diameter to surface area,
Percentage Diameter x y
Percentage diameter is another characteristic diameter which applies in common use.
Known as x y , it stands for the diameter x when the accumulative value of particle
size distribution is y%. With no special statement, y% is considered as the
accumulative value of weight (volume) distribution. Assuming it is a small-large
accumulation, for the sake of convenience, then x y can tell us that particles smaller
than x y cover y% of all the particles in the sample (see Picture A-3). Obviously
particles which are larger than x y cover (100-y)%.
Picture A-3
Usually we have x50 as the median diameter, which means that particles which are
smaller and larger than x50 respectively cover 50% of all. Occasionally it is also
used as the mean diameter. On most conditions, x50 is approximate to x(4,3) .
Obvious difference between x50 and x(4,3) indicates an extremely uneven size
distribution of particles.
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In many applications, the mean diameter and the width of the size distribution are
sufficient to provide an overall size information. According to different requirements
and habits, the mean diameter can be described by the volume mean diameter x(4,3) ,
the median diameter x50 , the particle amount mean diameter x(1,0) or the surface area
mean diameter x(3,2) . The width of the size distribution can be informed either by a
pair of boundary diameters, such as ( x10 , x90 ) , ( x 25 , x75 ) or ( x94 , x3 ) , or the standard
deviation according to statistics theories.
1
m m 2
σ ( p, q ) = ∑ ( xi − x( p, q )) 2 xi q ni /(∑ xi q ni )
i =1 i =1
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Authenticity
However, no ‘accuracy’ to standardize the size measurement of non-spherical particles
doesn’t mean the results can be given without proof. Variation in the measuring results
among different instruments should be within some reasonable tolerance, which is
called authenticity. So far the definition of ‘reasonable’ can only be found in some odd
theories instead of systematic researches. For instance, the measuring results of
standard particles by all particle size analyzers, regardless of what theories they apply,
should be within the acceptable error tolerance; the width of size distribution of
rodlike and flaky particles given by laser particle size analyzers should be within
theoretical ranges, etc. Opposite examples include: the highest range of
non-aciculiform particles analyzed by sieving even turns out to be 3-7 times larger
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than the diameter of sieve pore; particles of 1μm appear in the analysis report of
monodispersed standard spherical particles sized 10μm; Manufactures who boast their
instruments are available for particles of 0.1μm have no idea about what the Mie
scattering theory is, etc.
Repeatability
Repeatability is the relative deviation derived from multiple measurement reports on a
single sample by an instrument. The smaller the relative deviation is, the better the
repeatability is.
Provided that an instrument has k times of measurements on some physical quantity
with the respective values being v1 , v 2 ,......, v k , then the average value of the k
measurements should be:
k
V = ∑ vi / k
i =1
Specific surface area (SSA) is the summation of surface areas of all particles per unit
weight (volume) of sample powders.
When particles are regularly spherical, the volume specific surface area can be
calculated upon the size distribution. Provided that the diameter of a spherical particle
is xi , then its surface area is known as πxi and its volume as πxi / 6 . We have
2 3
i =1
i =1
i =1 i =1
m
= 6(∑ wi / xi )
i =1
where
wi = ni xi , i = 1,2,......, m is the weight distribution of particles and we have
3
∑wi =1
i =1
For non-spherical particles, the specific surface area derived from the above equation
is smaller than its real value and nevertheless can be modified by the shape coefficient
of particles.
Note that SSA derived from the above equation refers to the volume specific surface
area. Weight specific surface area is the value divided by the true density of sample.
Data Filing
variations (beyond the normal error tolerance) given by different instruments on the
same sample. Then how can users decide by which instrument and in which condition
the result is more accurate? How can they learn to compare among reports?
The following method has been proved practicable, i.e. saving the data by samples.
For self-consumed powders, save a certain volume (for example 10g) from the
certified samples and make sure the particle size data complies with the standard
when reproducing.
For commodity powders, send the certified samples to customers first and then
reproduce upon approval; otherwise find out the reason of disapproval, adjust the
technique to customers’ requirements and save the approved sample for reproducing.
Customers’ providing samples as compliance is also workable. Then we can conclude:
in particle size measurement, repeatability is the most essential factor.
Note that a mere information of particle size without that of the analyzing instrument
and the instrument manufacturer is invaluable for reference and even misleading
sometimes.
As is known, light is an electromagnetic wave. When light meets particles on its way
of traveling, the interaction between light and particles will result in deviations of part
of the light, which is called light scattering. See Picture A-5.
2
∞
2l + 1
Ia = ∑ {alπ l (cos θ ) + blτ l (cos θ )}
l =1 l ( l + 1)
2
∞
2l + 1
Ib = ∑ {blπ l (cos θ ) + alτ l (cos θ )}
l =1 l ( l + 1)
where
θ is the angle of scattering;
Ia is the scattered intensity of vertical polarized light of angle θ;
Ib is the scattered intensity of horizontal polarized light of angle θ;
where
1 4πσ c 2π
nˆ = (∈ +i ω= q= r
∈介 ω λ0 , λ介
), ;
∈介 is the dielectric constant of medium;
∈ is the dielectric constant of particles;
σ is the conductivity;
λ0 is the light wavelength in vacuum;
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πq
ϕ l ( q) = J 1 ( q)
2 l+
2
ζ l (1) ( q) = ϕ l ( q) + iχ ( q)
where
πq
χ l ( q) = − N 1 ( q)
2 l+
2 ;
J 1 ( q)
l+
2 is the Bessel function;
N 1 ( q)
l+
2 is the Neumann function;
l /2
( 2l − 2m )(l − 2m )
π l (cos θ ) = ∑ ( −1) m (cos θ ) l −2 m −1
m =0 2 m(l − m )(l − 2m )
l
1
= pl (cos θ )
(1)
sin θ
dπ l (cos θ ) d
τ l (cos θ ) = cos θπ l (cos θ ) − sin 2 θ = pl (cos θ )
(1)
d cos θ dθ
where
(1)
pl is the Associated Legendre Polynomial.
As it can strictly describe the scattered intensity of light, the Mie theory theoretically
applies for all kinds of particles. However, for large particles ( r 〉〉 λ ), its calculation is
very complex. Thus when calculating such large particles, diffraction formulas which
are simpler and more frequently used, will generally take the place. When particles
are infinitely far away from where they are observed, such diffraction formulas can be
simplified into the Fraunhoff equation as below:
A 2 J ( kr sin θ )
2
I (θ ) = (πr )
( )2 1 2 2
λf kr sin θ
Through observations, our R&D team has found that under the condition of r 〉〉 λ , the
Fraunhoff and Mie theories result in slight differences in displaying scattered light
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Assuming when there is no particle passing through the measurement window, the
light energy received by the central detector is E 0 and those by other detector elements
are E1 , E 2 ,L , E n in turn (due to aberration, dust scattering, etc.); when there are
particles in the window, the above light energies are represented
′ ′ ′ ′
by E 0 , E1 , E 2 ,L , E n , then
′
E − E0
Obs = 0
E0
That is called obscuration. The higher in concentration the sample is dispersed, the
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′
S i = Ei − (1 − Obs )Ei (i = 1,2,L , n)
represents the scattered light intensity distribution, which also indicates the size
distribution of particles being analyzed.
By photoelectric detectors, the received light energies are converted into relevant
current signals, which are magnified and realize the A/D conversion on the
data-collecting card before being finally sent to the computer.
Based on the light scattering theory and the optical structure of the instrument, the
computer has calculated in advance the scattered light intensity of each particle within
the measuring range and thus a model matrix is given as below:
m11 , m12 ,......, m1n
m , m ,......, m
2n
M = 21 22
....................
mn1 , mn 2 ,......, mnn
Each upright line in the above matrix symbolizes the scattered light intensity per unit
of weight per size class and we conclude:
• .................. •
sn mn1 , mn 2 ,......, mnn wn
where
w 1 ,w 2 ,…,w n is the weight distribution of sampled particles;
s 1 ,s 2 ,…,s n is the light intensity distribution of sampled particles.
Omit.
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Particle Diameter
Also called particle size, it symbolizes how big or small a particle is. Except for that
of spherical particles, particle diameter is an equivalent size which changes according
to different working theories of instruments, rather than a real physical size. In the
theory of light scattering which applies in particle size measurement, particle diameter
is considered as the diameter (distribution) of spherical particle (s) which has (have)
the same optical property and the most similar performance in light scattering as the
particles to be analyzed.
Distribution Mode
It’s the rule by which the sampled particles are distributed in size. There are four
models available in LS-909: General, Enhanced, Rosin-Ram and Single. General is
suitable for common samples, Enhanced mode is for wide –distribution samples,
Rosin-Ram (R-R), which is preferable for single-crest size distribution, and Single
mode is more applicable for monodisperse samples.
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Obscuration
Percentage or fraction of the illuminating light that is attenuated due to extinction
(scattering and/or absorption) by the particles. A large obscuration indicates a high
concentration of the sample.
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