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www.golighthouse.com Presentation Name Here
www.golighthouse.com Lighthouse Company Confidential: Do Not Distribute 060727A 1
Liquid Particle Counting Technology
And Applications
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Particle Measurement In Liquids
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Considerations for Liquid Particle Counting
Affects of Light Scattering in Liquids
Refractive Index
Flow Cell Design
Particle Counter Concentration Limits
Contamination
Bubble Formation
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Two Particle Detection Methods
1) Light Extinction (Light Blocking)
Attenuation of light signal. Measurement of particles
>1.0 micron
2) Light Scattering
Redirected light energy (Scattering) Measurement of
particles >0.05 micron
Particle Counting Basics
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Light Scattering In Liquids
Signal is a Function of the Ratio of Optical Index of Refraction of
the Particle to the Optical Index of Refraction of the Fluid
Considerations
Signal is smaller in Liquids
Fluid type affects signal in addition to particle composition
Flow Cell Design Affects the Background Noise of the Particle Counter (Quartz vs. Sapphire)
Particle IR
Media IR Signal =
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Some Important Indices of Refraction
Fluids Optical Index of Refraction @ 632nm (Red)
Air 1.0
Water 1.33
Hydrofluoric Acid 1.29
Sulfuric Acid 1.46
Ammonium Hydroxide 1.33
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Typical Optical Windows in Particle Counting
Material Optical Index of Refraction @ 632nm (Red)
Quartz (Fused) 1.458
Sapphire 1.7660
Quartz is Resistant to Many Chemicals, the Exceptions Being Hydrofluoric (HF)
Acid and Chemicals Containing HF
Sapphire is Resistant to Many Chemicals Including HF
Quartz has a Lower Index of Refraction then Sapphire, This Translates as Less
Reflective Energy Going Back into the Flow Cell, and Lower Background Noise
The Amount of Background Noise Affects the Liquid Particle Counters Sizing
Accuracy, and False Count Rates
This is Compounded by Contamination on the Flow Cell
For NON-HF Applications, Quartz is a Better Material then Sapphire as
Background Scatter is Less
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Particle Distributions
Liquid Distributions often Follow a 1/(diameter)3
Relationship in Fluids (Third Power Law)
Therefore There are 8 Times More 0.1 micron
Particles than 0.2 micron Particles in Such Fluids
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Particle Concentrations In Fluids Typical Particle Concentrations In Water
1
10
100
1000
10000
0.1 1 10
Particle Size (Microns)
Nu
mb
er o
f Par
ticle
s
Typical particle distributions follow an inverse 3rd power law, with more particles at
smaller sizes
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Flow Rate
Rate of Fluid Flow Through the Optical Cavity
“How Much Fluid” Flows THROUGH the Particle Counter
Defines the Transit time of Particle Through the
Sensor
A Function of the Capillary Cross Section
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View Volume View Volume is Defined by
the Amount of the Flow
Stream Illuminated by the
Laser
Full Stream (Volumetric)
Sensors have a View Volume of >80%
Partial Stream (In-situ)
Sensors have a Smaller View
Volume
Full Stream Particle Counter
Partial Stream Particle Counter
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Sample Volume
Flow Cell
Laser
View Volume
Sample Fluid
Sample Volume = Flow Rate x View Volume
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Optical Coincidence
Due to More Than One Particle Passing Through the Sensor at
a Given Time
The Reported Number of Particles is Less Than the Actual
Number of Particles (Coincidence Loss)
Coincidence Limit Decreases with Increased Sample Volume
Sensor View
Volume
Sensor View
Volume
Normal Operation
(One Particle in
View Volume)
Optical Coincidence
(More then One
Particle in View
Volume)
Inlet Flow Inlet Flow
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Bubbles
Bubbles are Detected as Particles
Pressure Can Be Used to Keep the Bubbles in
Solution so they are not Counted
On Line Applications use Head Pressure and back
Pressure Techniques to Eliminate Bubbles
Can Also use Differential Data and non-linear
Filtering Techniques to Eliminate Large Bubbles
from Data used for Process Control
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Liquid Particle
Counting Applications
(Online Sampling)
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High Purity Water Applications Clean water is important in many manufacturing operations
Semiconductor Device Fabrication
Flat Panel Display Fabrication
Disk Drive Media
Disk Drive Assembly
Pharmaceuticals
High purity water is used in cleaning, wet chemical processing, CMP
and immersion lithography
A few thousand gallons are used to process a single wafer
High purity water system contamination can directly contaminate product
Due to the importance of High Purity Water, these systems are monitored continuously for
particles and other types of contamination
Lighthouse Worldwide Solutions CONFIDENTIAL
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System Example: Real Time LPC Data
17
Optional software to display data on
company network.
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LMS Express RT Rolling Graph/Chart
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Online Measurement for UPW Systems
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Online Sampling of UPW
20
Remote Liquid Particle
Counter Sampling UPW with
Data Going to Laptop
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Online Measurement for WFI
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Low Particle Concentration Data
April 22 - April 25
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
0:00:00 2:24:00 4:48:00 7:12:00 9:36:00 12:00:00 14:24:00 16:48:00 19:12:00 21:36:00 0:00:00
Pa
rtic
les
pe
r m
L
0.1 micron
0.2 micron
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Hot UPW - 70C
0.00
0.20
0.40
0.60
0.80
1.00
1.20
1.40
1.60
1.80
2.00
1 8 15 22 29 36 43 50 57 64 71 78 85 92 99 106 113 120 127 134 141 148 155 162 169 176 183 190 197 204 211 218 225 232 239 246 253 260 267 274 281
(10 Minute Samples)
P/m
L
0.05 micron
0.1 micron
0.15 micron
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DI Data Spike (Second Pump Turns On)
0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
1 7 13 19 25 31 37 43 49 55 61 67 73 79 85 91 97 103 109 115 121 127 133 139
P/m
L
(10 Minute Samples)
Hot DI - Secondary Pump is Turned On
0.05 micron
0.1 micron
Secondary Pump
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In Situ Monitoring of Wet Benches
In Situ Particle Counting of:
Chemical Tanks (Etching, Plating, Cleaning)
Indication of Process Operations
Megasonic Cleaning Tanks
Indication of Process
Variables
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Bulk Chemical Delivery Systems
Particle Counts on Delivery Side of BCDS Systems
Bulk Chemical Delivery Quality Monitor
Loss Prevention for Wafer FAB
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Aqueous Cleaning
Very important in High Tech Manufacturing
Monitor Rinsing of Components, Media and
Sub-assemblies
Provides go/no go signal for processing
Provides end point signal for processing
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Industries that Require Precision Cleanliness Disk Drive Industry
Particles in the Drive Assembly Cause HDD Failure
Pharmaceutical Industry Particles in Injections can Cause Infections or Fever (Pyrogens)
Semiconductor Industry Particles in Tooling can Cause Device Failure
Aerospace Industry Particles Can Affect Components in Space Hardware
Machined parts Particles Cause Wear on Components
Pumps and Valves Particles will Cause Extensive Wear Leading to Failures or Clogging
Medical Device Industry Particles can Clog Syringes, Catheters, Valve Products
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Aqueous Cleaning System
Load
Table
Stage 1 CLEAN
•Ultrasonic
•Surfactant
•Overflow Bath
Stage 2 RINSE
Stage 3 FINAL RINSE Stage 4 DRY
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Baseline and Process Analysis Machine At Rest = 133 p/ml
Parts Final Rinse = 670 p/ml
Empty Baskets = 467 p/ml
The Baseline is calculated from the Average and the
Standard Deviation is used to understand the fluctuation
of the Baseline
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Liquid Grab Sampling
31
This is a pair of Liquid Grab Samplers
(LGS) connected to a rinse tank and
data going back to a PC.
LGS Close Up Picture
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Cleaning Process Optimization
0
200
400
600
800
1000
1200
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49 51 53 55 57 59
Series1
\
Tank
Water
Idle
Peaks Represent
Parts that have
Already Entered the
Tank
Valleys Represent Tank
Clean-up
Reference
Limit
Higher
Throughput
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Cleaning Process Optimization
0
200
400
600
800
1000
1200
1 3 5 7 9 11 13 15 17 19 21 23 2527 29 31 33 35 37 39 41 43 4547 49 51 53 55 57 59
\
New
Reference
Limit
Lower
Throughput
Cleaning
Tool
Idle
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Liquid Particle
Counting Applications
(Off Line or Lab Sampling)
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Liquid Particle Counting: Batch Sampling System
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High Purity Fluid Sampling
Batch Sampling Applications Allow Fluids to be Tested
for Purity
Samples of Production Chemicals / Fluids an be Tested
Laboratory Application to Support Production
Chemical Manufacturing
Quality Control
As Received Chemical Purity Testing
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Laboratory Parts Cleanliness Testing
Particles Contamination Affects:
Process Yield
Safety (Injectable Pharmaceuticals)
Long-term reliability (Component wear)
Product Performance and Customer Satisfaction ($)
Particle Contamination is Reduced by:
Precision Cleaning Operations
“Clean” Operations
Quantifying Parts Cleanliness by “Parts Testing”
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Parts Testing Data
Blank/Background
Post Clean Part Testing
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Pharmaceutical Applications:
USA
USP 30 <1> Injections
USP 30 <788> Particulate Matter in Injections
USP 30 <789> Particulate Matter in Ophthalmic Solutions
Europe
EP 5.7 (0520) Parenteral Preparations
EP 5.7 (2.9.19) Particulate Contamination: Sub-visible Particles
EP (0520) updated
Mandates particulate testing for SVI for human use–References EP 2.9.19 for test methods and limits–Excludes
radiopharmaceuticals–Suggests (but does not specify)
higher limits for intramuscular and subcutaneous
injections–Effective April 2005 [EP 5.1]
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Pharmaceutical Applications:
Japan
JP XIV General Rules
<11> Injections
JP XIV General Tests
<24> Insoluble Particulate Matter Test for Injections
<25> Insoluble Particulate Matter Test for Ophthalmic
Solutions
Korea
KP VIII
<52> Insoluble Particulate Matter Test for Injections
(Fundamentally a carbon-copy of the Japanese standards)
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Lab Application for LS-60
41
Engineer is testing a water
sample from their UPW
system.
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Liquid Products
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LS-20 Pharma Sampler
Easy Cleaning Via Sample Tube
Light-Blocking Design
USP 788 Compatible
Special USP Software Designed
to Enable 21 CFR Part 11
Compliance
Particle Range 1.0µm to 120µm
Various Ranges Available:
0.7µm– 120µm (BS) 1.0µm -120µm
1.0µm– 50µm (USP) 1.5µm - 400µm
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LS-60 Liquid Particle Counting: Sampling System
Syringe Sampling System
Beaker Size up to 1 Liter (1000ml)
Accommodates up to 50ml Syringes
Built In Stirring Mechanism with
Adjustable Speed
Adjustable Stage
Ranges:
0.1 to 0.5 micron
0.2 to 2.0 micron
0.3 to 3.0 micron
0.5 to 100 micron
1.0 to 400 micron
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Liquid Particle Counting: Online
Remote LPC 0.5
0.5 – 20 Micron
4 Channels
100 mL Flow Rate
Remote LPC 0.2
0.2 – 2.0 Micron
4 Channels
100 mL Flow Rate
Remote LPC 0.3
0.2 – 2.0 Micron
4 Channels
100 mL Flow Rate
Remote LPC 0.1
0.1 – 0.5 Micron
4 Channels
100 mL Flow Rate
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NanoCount 50+ and NC50C+ 50 Nanometer Detection
100 mL Flow Rate
5mL Sample Rate
Built in Color Display
View 4 Channels of Real Time
Data Locally
Integrated Flow Control
0.02 Counts/mL Zero Count Rate
Outputs: Ethernet, RS-485
MODBUS, 4 – 20mA
Hot DI Compatible
NanoCount 50+ Liquid Particle Counter
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NanoCount NC50C+ for Chemicals 50 Nanometer Detection
100 mL Flow Rate
5mL Sample Rate
Poly Propylene Casing
Integrated Flow Control with On-
Board Calibration Capabilities
0.02 Counts/mL Zero Count Rate
Outputs: Ethernet, RS-485
MODBUS, 4 – 20mA
Chemically Compatible
NanoCount 50C+ Chemically Compatible
Liquid Particle Counter
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30 Nanometer DI Water Technology 0.030um Particle Detection
4 Channel of Data
30nm, 50nm, 80 nm, 100 nm
Color Touch Screen Display
4 Channels of Data
Flow Status
Sample Time
Integrated Flow Meter
Flow Rate 80ml/min
Sample Rate 0.5ml/min
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25 Nanometer DI Water Technology 0.025um Particle Detection
4 Channel of Data
Color Touch Screen Display
4 Channels of Data
Flow Status
Sample Time
Integrated Flow Meter
Flow Rate 30ml/min
Sample Rate 0.5ml/min
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0.1 Micron Detection
Built in Degasser
Venturi Pump
Built in Flow Control
Built in Relay
Self Contained Package
Liquid Grab Sampler
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Summary
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Online Liquid Particle Counting Applications
- UPW (Ultra Pure Water)
- WFI (Water for Injection)
- Bulk Chemical Delivery Systems
- Parts Cleanliness Measurement
Batch Sampling (Laboratory Use)
- UPW (Ultra Pure Water)
- Process Chemicals
- Parts Cleanliness Measurement
- Testing of Injectable’s