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This presentation should not be considered a final statement of NIOSH policy or of any agency or individual who was involved. This information is intended for use in advancing knowledge needed to protect workers. Comments regarding this presentation may be submitted to the NIOSH Docket Office.

Cyrano Sciences

Array Based Chemiresistor Sensors for Residual Life and End of Service Life Indication

October 17, 2002

Product Platforms

CyranoseTM 320 NoseChipTM SensigentTM

DCS Data Decision Inputs

Wireless Sensors

Wireless Sensor Network Wireless Sensors

Front

Back

ANSWERS

Analysis Engine

· · · · ·

4 to 16 Sensors < 1 cm; Low Power Wireless Comm. to 300 ft Disposable Integrated Systems

Intelligent Sensor Networks

· Data Fusion

Handheld Point Detector / Identifier

Cyrano Sciences, Inc

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Cyrano Sensor Technology

Polymer Composite Sensor Array

Sensor Construction

Confining Wells Polymer Electrode 1 Insulating Layer Potentially Active Substrate Conductive Filler Electrode 2

Conductive Polymer Composite

Cyrano Sciences, Inc

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Cyrano Sensor Technology

Array Based Chemical Sensing

Vapors pass over the polymer composite sensors; swelling produces a change in resistance

Resistance change is measured for each of the 32 sensors

Using pattern matching algorithms, the data is converted into a unique response pattern

Cyrano Sciences, Inc

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Cyrano Sensor Technology

A resistive measurement is taken for each of the 32 sensors:

The vapor passes over the polymer matrix and the swelling produces a change in resistance

A relative resistance measurement is made for each of the 32 sensors

5

Cyrano Sciences, Inc

RLI Prototype Development

Cyrano RLI sensors

· disposable inside filter cartridge · intrinsically safety · sensor spot < 1 mm

sensors ~2 mm (in filter bed)

Alarm !

)

)

)

RLI %, unit ID, date & time

)

Cyrano RLI annunciator

· durable inside mask · wireless TX/RX power: micro Watts battery: weeks to > 1 year

Cyrano Sciences, Inc

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Cyrano NoseChipTM

Applications:

Individual Protection

· Filter RLI / ESLI - NIOSH · Personal badges - CBIRF

Collective Protection

Features:

· Sensor array; tunable · Low cost & Low power · Wireless communication · < 3 cm · Capable of integration

· Filter Monitoring in field shelters and buildings

Distributed Wireless Monitoring

· Permanent Installations (buildings) · Temporary Networks (events)

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Cyrano Sciences, Inc

Filter Breakthrough Testing

· Naval Research Laboratory ­ Comparison of sensor technologies for individual and collective protection · NIOSH ­ Contract awarded to Cyrano Sciences for prototype RLI for personal protective equipment · NASA ­ Detection of filter breakthrough detection in animal housing experiments

Cyrano Sciences, Inc

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Filter Breakthrough Testing

Naval Research Laboratory

· Comparison of Cyrano chemiresistor, SAW, PID and colormetric sensors · Challenge Vapor: DMMP · Cyrano's sensors perform as well as SAW sensors Fast, sensitive response · Internal testing shows Cyrano sensors use 300% less power than SAW sensors

Cyrano Sciences, Inc

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NRL Filter Breakthrough Tests*

Cyrano chemiresistor sensors are as sensitive and respond as rapid as SAW sensors

Cyrano Sciences, Inc

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NRL Filter Breakthrough Tests*

DMMP run 1-31-00 : CR 2 Data

11000 ? CR 2.1: 9000 ? CR 2.2: ? CR 2.3: ? CR 2.4:

Change in Resistance (Ohm)

7000

5000

3000

DMMP breakthrough

Date: 01/31/2000 Length of Trial: 9.00 hr Sample Rate: 10/min DMMP: 1500 mg/m3 (300 ppm) Flow rate = 10 Lpm. T = 300C %RH = House Air Sensor position: middle of 2.5 cm bed Breakthrough time @ 4000 sec.

1000

Data from NRL

0 2000 4000 6000 8000 Time (sec) 10000 12000 14000 16000

-1000

R. Andrew McGill

Cyrano chemiresistor technology successfully used as Filter Breakthrough/Residual Life Indicator

Cyrano Sciences, Inc

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NIOSH RLI for Air Purifying Respirators

· Contract awarded for further development of Residual Life Indicator (RLI) technology. · 3 part program includes: · Determination of detection limits and sensor selection · Filter breakthrough detection · Development of prototype mask/detector system · One year program; prototype detector systems delivered June 2003

Cyrano Sciences, Inc

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Determination of Detection Limits

· Determine detection limit of 10 VOC's chosen by NIOSH using system illustrated below · Select sensors for breakthrough testing by "ranking" them according to detection limit to different chemical families

Gas Dilution System Sensor Test Cell Exhaust/ Scrubber

Analyte and Air Tanks

Mixture Control

Data Acquisition

Cyrano Sciences, Inc

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MDL Studies for TICs, CWA

Ammonia SNR > 100 at REL 25 ppm Nitrogen Dioxide SNR > 400 at REL 3 ppm Phosgene SNR > 10 at REL 2 ppm

700 600

400 350

CEES

500 400

300 250

DMMP

SNR

SNR

200 150 100 50 0

300 200 100 0

0 2 4 6 8 10

0

0.05

0.1

0.15

0.2

Concentration (ppm)

Concentration (ppm)

Cyrano Sciences, Inc

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NIOSH Filter Breakthrough Test Bed

sensor array sensor array Vapor Flow

10 ­ 50 Lpm

#1

#2 1.5"

#3 1"

3"

3M NIOSH 7251 OV cartridge

GC sample

GC sample

A schematic representation of the RLI test fixture

Cyrano Sciences, Inc

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NIOSH Filter Breakthrough Test Bed

Cyrano Sciences, Inc

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NIOSH Vapor Generation System

Capabilities

· Concentration: <1 ppm to Saturation · Flow Rate: 0.1 to 100 Lpm · Solvents, TICs, CWA simulants · Mixtures

Cyrano Sciences, Inc

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Multi-Filter Breakthrough ("RLI")

0.018 1.8%

Single 4hr test: 10/15/02 Filter #1 Filter #2

Normalized Resistance Change

0.016 0.014 1.4% 0.012 0.01 1.0% 0.008 0.006 0.6% 0.004 0.002 0.2%

5400 ppm sensors s1,s2 on array #1 sensors s1,s2 on array #2 50 ppm

3000 5000 7000 9000 11000 13000

0% 0

1000 -0.002

Time (sec)

Cyrano Sciences, Inc

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Challenge concentration 6000ppm

NIOSH Filter Breakthrough Test Bed

sensor array sensor array Vapor Flow

10 ­ 50 Lpm

#1

#2 1.5"

#3 1"

3"

3M NIOSH 7251 OV cartridge

GC sample

GC sample

A schematic representation of the RLI test fixture

Cyrano Sciences, Inc

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Breakthrough Event Detection

0.8%

Normalized Resistance Change

Filter #1

0.6%

Concentration at breakthrough confirmed by GC (ppm)

5400 5650

0.4%

3500 750 50

chemiresistors record event

s5 s9 s23 s29

0.2%

0.0% 1000.0

3000.0

5000.0

7000.0

9000.0

11000.0

13000.0

60 70 80 90 100 (minutes)

-0.2%

(sec)

Time

Cyrano Sciences, Inc

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Breakthrough Event Detection

0.8%

Filter #1

Normalized Resistance Change

0.6%

Filter #2

s5 s9 s23

0.4%

s29

0.2%

0.0% 1000

3000

5000

7000

9000

11000

13000

-0.2%

Time (sec)

Cyrano Sciences, Inc

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NIOSH Recommended Filter Challenge Vapors

Test Breakthrough Conc. (ppm) draft 10 12.5 1 1.25 0.3 2 4.7 5 5 1

Cyrano Sciences, Inc

Challenge Chemical

Cyclohexane Ammonia Formaldehyde Phosgene Phosphine Cyanogen Chloride Hydrogen Cyanide Hydrogen Sulfide Sulfur Dioxide Nitrogen Dioxide

Conc. (ppm) draft 3900 2500 500 250 300 300 1000 940 1500 200

RLI IDLH 8-hr TWA Detector Reqt. (ppm) (ppm)

REL / TLV 1300 300 20 2 50 n.a. 50 100 100 20 300 25 <1 0.1 0.3 0.3 4.7 10 2 3 ? ? ? ? ? ? ? ? ? ?

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