HELOS Laser Diffraction - 0.1 M To 8,75 MM: Better Particles With Best Instruments

Better Particles with Best Instruments
HELOS Laser Diffraction| 0.1 µm to 8,75 mm
HELOS-RODOS/M TRAINING
M16 & Eagle Nebula © Johannes Schedler | Panther Observatory

© Copyright 2014-16, Sympatec GmbH, D-38678 Clausthal-Zellerfeld, Germany | QICPIC & Co. Image Analysis | 16T01R06M1EN
Topics
• Fundamentals of particle size analysis and laser diffraction

• HELOS system hardware components
• HELOS system WINDOX control software
• Measurement setup
• Handling of results
• Automation and custom reporting tools
• WINDOX Administrative functions
• Database and User management
Modern Techniques of Particle
Characterization
 Sympatec brings to market instruments based on the following methods:

 HELOS | Laser diffraction OPUS | Ultrasonic extinction
» Particle size distribution Particle size distribution and
» 0.1 µm to 8,750 µm concentration
 QICPIC | Dynamic image analysis < 0.1 µm to 3,000 µm
» Particle size and… shape NANOPHOX | PCCS

distribution Particle size distribution and stability
» < 1 µm to 34,000 µm 0.5 nm to 10,000 nm
 Our instruments provide the following advantages

compared to legacy PSA techniques such as sieving:
• Much greater sensitivity • Fast
• High statistical relevance • Versatile
• Wide dynamic range
Sensor Technologies
Measuring Ranges
< 1 µm Dynamic Image Analysis | Size and Shape 34,000 µm
0.1 µm Laser Diffraction | Size 8,750 µm
< 0.1 µm Ultrasound Extinction | Size and Concentration 3,000 µm
0.5 nm PCCS* | Size and Stability 10,000 nm
*Photon Cross Correlation Spectroscopy

0.0001
0,1 nm 0.001
1 nm 0.01
10 nm 0.1
100 nm 11
µm 10µm
10 100µm
100 1000
1 mm 10000
10 mm 100000
100 mm
Particle Characterization
„Best Practice“
 Best possible analysis

results request
Analysis Result
» Representative sampling
» Dispersion to the
Instrument
Dispersion
primary particles
Analytical
Sampling
» Effective instruments for
precise measurement and
evaluation | analysis
Particle Characterization
Error sources | Schematic
1000
Dispersion
Sampling
100
Error / %
10
Technology-dependent
Analytical instrument
0.1
0.01 0.1 1 10 100 1000 10000
Particle Size / µm
In reference to Henk G. Merkus (1997), TU Delft
Extraction of a Sample for Analysis
Sample Taking | Sample Splitting
 Crucial for representative

measurement results
 Representativity
determined by
» Sample size
» Number of subsamples
» Particle size
» Width of distribution
Extraction of a partial sample

» Segregation behaviour
© markadan wikicc
Representative Sample Splitting
Laboratory
 Increasing the number of partial samples z decreases the

error influence e | e²  1/z
 Dynamic splitting
» Rotating riffler
» z large | small error
product feed
vibrating chute
mass flow
turning carousel rotation
THE HELOS-RODOS/M-VIBRI SYSTEM
HELOS = sensing device
VIBRI = dosing device
RODOS = dispersion device

HELOS - RODOS | Dispersing Systems
Dry Dispersion
RODOS/L | Free aerosol jet
VIBRI | Precision Vibratory Chute
Continuous Sample Mass Flow
VIBRI
 Provides a precise constant sample mass
flow to the RODOS dispersion module
 Rotating funnel and hammer add-on
provide automated cleaning of sticky
powders
RODOS | Unrivalled Dry Disperser
Reproducible Dispersion Effect
Air flow rate

No re-agglomeration or deposits
up to 200 l/min
Powder Venturi restriction creates a depression
introduction
Straight Particle Stream formation
Free
acceleration section Mixing zone
aerosol jet
Without | with baffle cascades vmax> 200 mi/hr
Adaptable dispersion
energy via primary
pressure and ring gap
(Venturi restriction)
Dry Dispersion
Dispersion Principle | Injection
Dispersion with Compressed Air* Principle

» Velocity gradients
» Collisions between particles
» Collisions between
particles and wall
*variable adaptation of the dispersion energy to the product requirements
HELOS | Sensor Family
BR | KR | Dry and Wet
HELOS/BR 0.1 µm – 875 µm HELOS/KR 0.1 µm – 8,750 µm
QUIXEL GRADIS
HELOS/KR 0.1 µm – 8,750 µm HELOS/KR-Vario 0.1 µm – 8,750 µm
OASIS/M Variable measuring zone up to > 2 m
HELOS
Optical Setup
Dispersion Module Optical Detector

module
Beam
expander
He-Ne Laser light

source
Particle flow
Measuring
zone
* ISO 13320, § 5, fig. 2 for particle size from 0.1 µm to approx. 3.0 mm
Laser Diffraction | Principle
Interactions | Particle and Laser Light Waves
Fraunhofer Diffraction | diffraction (no parameters required)
Θ
Θ Θ
The diffracted light creates a unique Large particles

Absorption Small diffraction
x interference pattern that is
dependent on the size of the angles
Θ
particles
Θ Θ
Plane light wave e.g.

parallel laser beam Reflection Refraction
Mie Scattering | diffraction + reflection + refraction + absorption Small particles

(complex refractive index required) Large diffraction angles
HELOS – Laser diffraction sensor
HELOS sensing principle: Forward Scattering (Fraunhofer Diffraction)
HELOS detector compartment
• 31 semi-circular elements for

Scattered Intensity profile
• 3-sector central element for

detector alignment (auto-focus)
perfectly centered
laser beam
Size Distribution from Scattered Intensity
31-element intensity profile 31-bin cumulative size distribution curve
HELOS | Measuring Ranges
Optics Revolver
Automatic change of
measuring ranges
Software-controlled | SOP
Resolution adapted to the Product
 Individual optical modules adapt the measuring range to the sample

» Optimum resolution in the area where it is needed
» Fraunhofer evaluation of submicron-particles with
special short focal distance optics
» Reliable detection of large particles with long focal distance
» Range combination with all advantages – including very broad
distributions
0.1 µm to 8,750 µm with Maximum Resolution
R8 0.5 first class 45 MEGAMICRON f‘=5,000 mm 8,750
R7 0.5 18 TOPMICRON f‘=2,000 mm 3,500
R6 0.5 9 TOPMICRON f‘=1,000 mm 1,750
R5 0.5 first class 4.5 (TOPMICRON) f=500 mm 875

KR
R4 0.5 1.8 (TOPMICRON) f=200 mm 350
R3 0.5 0.9 Fourier lens f=100 mm 175 BR
R2 0.25 0.45 SUBMICRON f=50 mm 87.5
R1 0.1 0.18 SUBMICRON f=20 mm 35
0.1 1 10 100 1000 10000

Particle Size / µm
HELOS | Laser Diffraction
Range Combination
 For samples with wide

distributions
R7  Maximum measuring range

R5 from 0.1 µm to 8,750 µm
R3
 High resolution, precise
R1 individual analysis in parallel
laser beam
 Parameter-free over the
complete range with
Intensity distribution on
virtual detector
Fraunhofer
 Mie if accurate optical
properties are known
 No combination of different
measuring principles or
multiple detectors needed
Particle Size Distribution
Cumulative Distribution
100
Q3(xmax)= 100 % | xmax
90
90 % ≤ x90=33.47 µm
Cumulative Distribution Q3(x) / %
80
70
60
Reading point 23
50
50 % ≤ x50=15.90 µm 70.17 % ≤ x70,17=21.5 µm
Mean particle size
40
30
20
10
Q3(xmin)= 0 % | xmin 10 % ≤ x10=7.23 µm Cumulative curve
0
0.1 1 10 100
Particle Size / µm
Distribution Density | Mono-modal
100 1.6
Mode Cumulative curve
90
52.5 % ≤ xD≈16.4 µm 1.4
80
1.2
Density Distribution q3*

70
The density curve represents the The area underneath the 1.0
60
gradient of the cumulative curve density curve equals 1
50 ( ) 0.8
∗
= lg =
40
lg
0.6
30
0.4
20
0.2
10
Frequency distribution Density curve
0 0.0
0.1 1 10 100
Particle Size / µm
Cumulative and Density Distribution | Bimodal
100 1.8
Coffee Powder Mode 1 Cumulative curve
90 1.6
64.2 % ≤ xD,1≈436 µm
80
x99.98 = 1220 µm 1.4
Distribution Density q3*

70
1.2
60
1.0
50
50 % ≤ x50=355.48 µm 0.8
40
0.6
30
Mode 2
20
9.2 % ≤ xD,2≈49 µm 0.4
x0.06 = 11 µm
10 0.2
Density curve
0 0.0
1 10 100 1000
Particle Size / µm
Measurement Results | Two Batches
Reproducible | Comparable | Sensitive
100
Sample x(10%) x(50%) x(90%)
90 µm µm µm
 Cement_#1_01 1.29 12.19 42.66
80  Cement_#1_02 1.30 12.24 42.81

 Cement_#1_03 1.30 12.26 43.13
70  Cement_#2_01 1.26 11.84 41.42
 Cement_#2_02 1.26 11.80 41.25
60  Cement_#2_03 1.26 11.81 41.30
50
40 69
30 64
20 59
54
10
10 20
0
0.1 1 10 100
Particle Size / µm
WINDOX Software
Instrument control
HELOS sensor control software module
Database and User

administration modules
Copyright 2011, Sympatec Inc.

1600 Reed Rd., Suite C, Pennington, NJ 08534
Database administration module
Main functions:
• Create new database
• Register/Unregister existing database
• Database maintenance
• Restore archive of selected measurements

User administration module
• Based on MS-WINDOWS user access

• Can fine tune individual use/access rights of WINDOX modules
HELOS Sensor Control
From here we can control all of the

functions required to perform a
measurement, Product, Measuring
range, Trigger condition and
Disperser.
Once each of these conditions is

fulfilled we are able to perform a
measurement.

HELOS Sensor Control
The most important settings. If one

of these is empty, there will be no
measurement!

Key features of sensor Control
Window
Shows currently selected measurement and

opens database browser
Opens signal test Window
Save, Save As, Undo, Delete

Note – any changes made must be saved
before the measurement in order to take effect.
Changes lower half of sensor control window to

show settings for selected icon. In this case
Trigger condition is selected.

Database browser tools
Opens preferences screen to change view in the main database browser
Loads selected measurement from database into Sensor Control.
Evaluates selected measurements according to WINDOX settings, use Shift/Ctrl to select

multiple measurements
Create an archive of selected measurements

Database filters – selection of measurements
Standard Filter
Expert Filter

Exporting of measurements
Select the measurements you wish to export and click on
Then select a folder for the measurements to go into. This archived file can then be
recovered using the database administration program.

Combing measurements (Range Combination)
The measurements selected must match the following requirements:
• data acquired by the same HELOS instrument
• exactly one measurement per measuring range
• the gap between two measuring ranges to be combined should not be larger than 3
Select the measurements you wish to combine and click on

Signal Test Window
• Monitor optical
concentration values in
measurement area
• Switch between live
mode and saved stream
database mode
• Perform Auto-focus

Product page

Trigger setup page
Sets criterion for when conditions are valid

for measurements and start stop triggers

Dispersing setup page
Sets disperser type and adjustable parameters

Evaluation and Output
Use this screen to control how you want to view

the data after measurement
There are 3 principal ways to view data in the

WINDOX software,
Report Template Editor
Report
Distribution diagram

Editing the distribution diagrams
Right click on the Legend box to open the

legend data this will give you access to the
same commands as in the Report Editor – this
allows you to add any of the commands in the
list to the distribution diagram.

Template Editor Functionality
Controls which report is

selected for output, either on
screen or to be printed, can
also use to select statistical
reports.
Opens the report template

command list.
Unlocks the selected report for

editing.
Report Editor – command list
The above icon opens the

report template command
list. Use this to add new
features or commands to a
report. Adding the xi
command shown to the
side would generate the
command @xi.(50,3) that
will display the x50
diameter of the volume-
based distribution.

Report Editor – embedding calculations within a report

Report Editor – Common commands

Report Editor – List of template commands under WINDOX help

Report Editor – Full list and syntax of data values under WINDOX help

Report Editor – Full list and syntax of data values (cont’d)

Report Editor – Size distribution example template
report_QICPIC_Q3_CD

Report Editor – Size distribution output of example template
Sympatec GmbH
System-Partikel-Technik QICPIC Particle Size Analysis
WINDOX 5
QICPIC (QP0207) & RODOS/L, 1.00 63.0 mm - M7 (5 ... 2688 µm)

2015-11-24, 12:11:44,787
x10 = 409.78 µm x50 = 597.31 µm x90 = 884.40 µm SMD = 552.13 µm VMD = 629.33 µm
x16 = 443.09 µm x84 = 823.14 µm x99 = 1235.94 µm
100 3.25
3.00
90
2.75
80
Cumulative distribution Q3 / %
2.50
Distribution density q3*

70 2.25
60 2.00
1.75
50
1.50
40 1.25
30 1.00
0.75
20
0.50
10
0.25
0 0.00
10 50 100 500 1000 5000 10000
Particle size / µm
cumulative distribution
x0/µm Q3/% x0/µm Q3/% x0/µm Q3/% x0/µm Q3/%
7.90 0.00 84.86 0.28 874.54 89.60 9013.22 100.00
10.00 0.00 103.06 0.36 1062.19 97.24 10947.26 100.00
12.15 0.00 125.18 0.46 1290.12 99.55 13296.29 100.00
14.75 0.00 152.04 0.57 1566.95 99.97 16149.37 100.00
17.92 0.01 184.66 0.70 1903.18 100.00 19614.66 100.00
21.76 0.01 224.29 0.87 2311.55 100.00 23823.51 100.00
26.43 0.02 272.41 1.23 2807.56 100.00 28935.50 100.00
32.10 0.04 330.87 2.58 3410.00 100.00 34100.00 100.00
38.99 0.07 401.86 8.57 4141.71 100.00 49625.41 100.00
distribution density (log.)
xm/µm q3lg xm/µm q3lg xm/µm q3lg xm/µm q3lg
5.59 0.00 77.00 0.01 793.53 1.99 8178.38 0.00
8.89 0.00 93.52 0.01 963.81 0.90 9933.28 0.00
11.02 0.00 113.58 0.01 1170.62 0.27 12064.74 0.00
13.39 0.00 137.96 0.01 1421.81 0.05 14653.55 0.00
16.26 0.00 167.56 0.01 1726.90 0.00 17797.87 0.00
19.75 0.00 203.51 0.02 2097.45 0.00 21616.89 0.00
23.98 0.00 247.18 0.04 2547.51 0.00 26255.39 0.00
29.13 0.00 300.22 0.16 3094.15 0.00 31411.79 0.00
35.38 0.00 364.64 0.71 3758.09 0.00 41136.68 0.00
evaluation: WINDOX 5.9.0.0 product: Aproduct

calculation mode: FERET_MEAN density: 2.7100 g/cm³
class limits: M7 Copt: 0.22 %
trigger condition: 500hz full 5s oco0.05% 20s 5.. user parameters:

start: c.opt >= 0.05% Customer: Acustomer
valid: always Identifier: 2
stop: 20s c.opt <= 0.05% or 500s real time Sample splitting: yes

Report Editor – Display individual measurement values in a statistics report

Report Editor – Import/Export .wxr templates

WINDOX automation
• Offline (HELOS) and Online (MYTOS, MYTIS) versions
of the instruments share the same core hardware
components
• A very robust software suite, WINDOX, was developed
to support all needs, including remote communication
HELOS and automation functions
MYTOS
MYTIS
• Heart of WINDOX system is an “Application Server” module

• It interfaces the Databases to the Instrument Control and Data
Visualization modules
• Users can write programs to automate the operation of the Application
Server
WINDOX automation: Application Editor


HELOS Laser Diffraction - 0.1 M To 8,75 MM: Better Particles With Best Instruments

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Better Particles with Best Instruments

HELOS Laser Diffraction| 0.1 µm to 8,75 mm

M16 & Eagle Nebula © Johannes Schedler | Panther Observatory

• Fundamentals of particle size analysis and laser diffraction

 Sympatec brings to market instruments based on the following methods:

 QICPIC | Dynamic image analysis < 0.1 µm to 3,000 µm

» Particle size and… shape NANOPHOX | PCCS

 Our instruments provide the following advantages

< 1 µm Dynamic Image Analysis | Size and Shape 34,000 µm

0.1 µm Laser Diffraction | Size 8,750 µm

< 0.1 µm Ultrasound Extinction | Size and Concentration 3,000 µm

0.5 nm PCCS* | Size and Stability 10,000 nm

*Photon Cross Correlation Spectroscopy

 Best possible analysis

 Crucial for representative

Extraction of a partial sample

 Increasing the number of partial samples z decreases the

turning carousel rotation

HELOS = sensing device

VIBRI = dosing device

RODOS = dispersion device

RODOS/L | Free aerosol jet

Air flow rate

Without | with baffle cascades vmax> 200 mi/hr

Dispersion with Compressed Air* Principle

» Collisions between particles

*variable adaptation of the dispersion energy to the product requirements

HELOS/BR 0.1 µm – 875 µm HELOS/KR 0.1 µm – 8,750 µm

OASIS/M Variable measuring zone up to > 2 m

Dispersion Module Optical Detector

He-Ne Laser light

Fraunhofer Diffraction | diffraction (no parameters required)

The diffracted light creates a unique Large particles

Plane light wave e.g.

Mie Scattering | diffraction + reflection + refraction + absorption Small particles

HELOS sensing principle: Forward Scattering (Fraunhofer Diffraction)

• 31 semi-circular elements for

• 3-sector central element for

31-element intensity profile 31-bin cumulative size distribution curve

 Individual optical modules adapt the measuring range to the sample

R8 0.5 first class 45 MEGAMICRON f‘=5,000 mm 8,750

R7 0.5 18 TOPMICRON f‘=2,000 mm 3,500

R6 0.5 9 TOPMICRON f‘=1,000 mm 1,750

R5 0.5 first class 4.5 (TOPMICRON) f=500 mm 875

R3 0.5 0.9 Fourier lens f=100 mm 175 BR

R2 0.25 0.45 SUBMICRON f=50 mm 87.5

R1 0.1 0.18 SUBMICRON f=20 mm 35

0.1 1 10 100 1000 10000

 For samples with wide

R7  Maximum measuring range

Density Distribution q3*

Distribution Density q3*

80  Cement_#1_02 1.30 12.24 42.81

Database and User

Copyright 2011, Sympatec Inc.

Copyright 2011, Sympatec Inc.

• Based on MS-WINDOWS user access

From here we can control all of the

Once each of these conditions is

Copyright 2011, Sympatec Inc.

The most important settings. If one

Copyright 2011, Sympatec Inc.

Shows currently selected measurement and