Liquid Particle Counter Applications · The Amount of Background Noise Affects the Liquid Particle Counters Sizing Accuracy, and False Count Rates . This is Compounded by Contamination

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Liquid Particle Counting Technology

And Applications


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Particle Measurement In Liquids



Considerations for Liquid Particle Counting

Affects of Light Scattering in Liquids

Refractive Index

Flow Cell Design

Particle Counter Concentration Limits

Contamination

Bubble Formation



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



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 =



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



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



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



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



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



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



Sample Volume

Flow Cell

Laser

View Volume

Sample Fluid

Sample Volume = Flow Rate x View Volume



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



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



Liquid Particle

Counting Applications

(Online Sampling)



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



System Example: Real Time LPC Data

17

Optional software to display data on

company network.



LMS Express RT Rolling Graph/Chart



Online Measurement for UPW Systems



Online Sampling of UPW

20

Remote Liquid Particle

Counter Sampling UPW with

Data Going to Laptop



Online Measurement for WFI



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



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



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



Bulk Chemical Delivery Systems

Particle Counts on Delivery Side of BCDS Systems

Bulk Chemical Delivery Quality Monitor

Loss Prevention for Wafer FAB



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



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



Aqueous Cleaning System

Load

Table

Stage 1 CLEAN

•Ultrasonic

•Surfactant

•Overflow Bath

Stage 2 RINSE

Stage 3 FINAL RINSE Stage 4 DRY



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



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



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



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



Liquid Particle

Counting Applications

(Off Line or Lab Sampling)



Liquid Particle Counting: Batch Sampling System



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



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”



Parts Testing Data

Blank/Background

Post Clean Part Testing



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]



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)



Lab Application for LS-60

41

Engineer is testing a water

sample from their UPW

system.



Liquid Products



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



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



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



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



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



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



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



Summary



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



Thank You

Documents

Liquid Particle Counter Applications · The Amount of Background Noise Affects the Liquid Particle Counters Sizing Accuracy, and False Count Rates . This is Compounded by Contamination