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Bob Hughes-FTSCPACMark LaPrevotte-FTSCLANT

Cleaning Oxygen and Diver’s Breathing Air Instruments

Eliminating Ozone Depleting Solvents

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Background• Navy OICR’s clean oxygen

Instrumentation with CFC-113 solvent and verify cleanliness with Infrared (IR) Spectroscopy

• CFC-113 solvent is an Ozone Depleting Solvent that stopped manufacture in 1996 IAW the Montreal Protocol

• CFC-113 is stockpiled in the DoD Mission Critical Reserve

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Stockpile• Initially sized for 2 years to “buy time”

until alternative in place

• Sizable stockpile remains due to late purchase, conservation, and use of replacement solvents for other applications

• Some estimates indicate it could last at least 10 years

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Stockpile• The life span may be reduced to 4 to 5 years

based on:– USAF may replace HCFC-141b in spray cans with

CFC-113 due to near-term future use restrictions (2000 gallons annually)

– One LOX producer has required partial flushing in the last 4 years. A complete flush uses 1500 gallons

– Resources to maintain stockpile indefinitely have not been programmed

– Quality problems

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Stockpile PolicySupply CFC-113 until it is depleted, at

which time approved alternative

replacement solvents will be substituted

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HFE-7100• Replacement oxygen instrument cleaning

solvent for CFC-113

• No ozone-depleting potential

• Toxicity similar to CFC-113

• No compatibility problems

• Can be used with existing cleaning and atmosphere monitoring equipment

• Quality product available per A-A-59105

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HFE-7100 • Cleaning Performance - Dissolving and

Displacement– Marginal hydrocarbon solvency– Excellent fluorocarbon solvency– Excellent removal by displacement due to low

surface tension and high density– NASA testing showed for instrument cleaning,

HFE-7100 removed 92% of soil and CFC-113 removed 97%

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Cleanliness Verification - IR• IR analysis is usable ONLY with solvents

that are transparent in the C-H Stretch Region

• All approved replacement solvents (HCFC-141b, HCFC-225, and HFE-7100) are not verifiable with IR

• Unlikely that other candidate solvents will be verifiable with IR

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• Industry standard is Non-Volatile Residue (NVR) by Evaporative Gravimetrics

• NVR usable with any solvent

• NVR requires 75 to 100 ml sample

• Takes 2 hours per analysis

• Must be performed in a Chemistry Laboratory

Cleanliness Verification - NVR

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• Optically Stimulated Electron Emission (OSEE) is newly developed alternative analysis technique

• OSEE usable with any solvent

• 1.5 ml sample taken as gage is cleaned

• Performed on-site in OICR in about 20 minutes

• Replaces NVR and implemented at NASA

Cleanliness Verification - OSEE

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OSEE Synopsis• An instrument shines an ultraviolet light on

a surface and measures the electrons emitted from the surface. As the surface is more soiled, it will emit less light (electrons).

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OSEE Synopsis (Cont’d)• An evaporating dish is hand cleaned with

detergent. This dish holds the solvent. After the solvent evaporates, it leaves residue behind. This residue is compared to the residue remaining from a 5 ppm standard to determine if it is above or below 5 ppm.

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Equipment The equipment easily fits into OICR

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On-Site Testing (Past and Proposed)• Testing has been accomplished at PSNS

and NASA for the last 2 years

• Perform additional on-site testing at minimum of two facilities (other than PSNS), one under FTSCPAC and the other under FTSCLANT, for one year

• Clean with CFC-113 and analyze with IR and OSEE

• Closely monitor testing and get input

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• Equipment will be provided to activities that request the equipment and agree to use the equipment (limited quantities)

• Operation of equipment will be verified and sampling line will be oxygen cleaned

• Equipment will be assembled into a kit and shipped (limited quantities)

• Training will be provided by Bangor, WA when established

• Bangor, WA will provide 5 ppm standards

Implementation

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Implementation

• Facilities can clean with CFC-113 and analyze using both IR and OSEE to gain confidence and familiarity with OSEE

• Once comfortable with OSEE, it is the option of the facility to use CFC-113 with IR and/or OSEE or HFE-7100 with OSEE until stockpile depleted

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• A new manual for Instrument and Gage Cleaning for MIL-STD-1330 (-) Applications will be generated

• Currently usable by NAVSEA Facilities, Vendors, and Foreign Military

When will this happen?

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Why do we need to do this?• The stockpile is not programmed to last

“forever”

• A change of events could deplete it rapidly

• IR can not be used for new oxygen cleaning solvents

• It aligns the Navy with Industry (currently we use IR and industry uses NVR)

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Why do we need to do this?• The Navy has been directed to eliminate

the use of Ozone Depleting Solvents

• Implementing an alternative starting now and over a period of 5 years will ease the transition

• It is inevitable

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Diver’s Breathing Air Instruments

• MIL-STD-1622(B): Appendix C added to address diver’s air breathing instruments. Status: At NAVSEA for approval

• UIPI 5510-905(-): New UIPI for cleaning diver’s air breathing systems, including instruments. Status: Has been issued

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Calibration Only-No Cleaning• Installed Instrument

– Used exclusively in Diver’s breathing air or cleaner application

• New or previously cleaned and not installed– Sticker or tag indicating cleaned per MIL-

STD-1622 or equal

• Properly packaged

• Internals pass visual inspection

If any of these not met, cleaning is required

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Cleaning and Calibration• Pre-cleaning and final cleaning

– Inspection of internals reveals other than particulate

• Final cleaning only (pre-cleaning not required)– Inspection of internals reveals only particulate

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• Pre-cleaning– Apply pre-cleaner (HFE-71DE or CFC-

113) using any method such as a syringe

– Rotate instrument to wet internals

– Repeat until 10 ml is obtained

– Visually inspect effluent

– Repeat until passes visual inspection

Cleaning Procedures

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• Final Cleaning– Option 1:

• Repeat precleaning except use final cleaner (HFE-7100 or CFC-113)

• Perform final cleaning once for instruments that hold less than 10 ml and twice for instruments that hold more than 10 ml

Cleaning Procedures

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• Final Cleaning– Option 2:

• Final clean per NAVSEA ST700-AM-GYD-010/OICR except use dedicated equipment

• Analysis for organic cleanliness verification (hydrocarbons) is not required

Cleaning Procedures

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NEW TECHNOLOGY

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Fast

Rugged

Automated

Small Sample Size

NanoScale 9100

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Run more samples in less time

Easy to run verification samples

Average run time is 5 to 7 minutes

FAST

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No vibration isolation required

Office type environment acceptable

Easily transported

RUGGED

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Reduces human error

Can be integrated with other tasks

Highly skilled operators not required

Automated

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Greatly reduces emissions

Reduces cost of analysis

Greatly reduces depletion of a bath in

a production QC application

SMALL SAMPLE SIZE

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Log sample information

Acquire sample

Inject sample

Record results

Clean to prepare for next sample

SIMPLE TO OPERATE

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Log Sample Information

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Acquire Sample

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Acquire Sample

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Acquire Sample

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Acquire Sample

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Acquire Sample

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Fast, rugged, automated, small sample

size

Simple to operate

Unique Flexural Plate Wave (FPW)

gravimetric sensor

Nanogram sensitivity

SUMMARY

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Direct readout in mass or

concentration

Reduces total laboratory emissions

NVR measurement in as little as 5

minutes

Variety of applications

SUMMARY (Con’t)

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Company incorporating recommended

improvements

Technology “new” in industry less

than one year

NASA doing evaluation

Possible Navy evaluation

CURRENT STATUS