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An atomic fluorescence-based, reagent-free, field-deployable mercury analyzer

An atomic fluorescence-based, reagent-free, field-deployable mercury analyzer. Joel Creswell, Ph.D. Technical Director. Background. Problems with field monitoring of mercury: Sampling is expensive Handling causes contamination Samples must be transported Cost & effort limits frequency

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An atomic fluorescence-based, reagent-free, field-deployable mercury analyzer

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  1. An atomic fluorescence-based, reagent-free, field-deployable mercury analyzer Joel Creswell, Ph.D. Technical Director

  2. Background • Problems with field monitoring of mercury: • Sampling is expensive • Handling causes contamination • Samples must be transported • Cost & effort limits frequency • Unmet research needs: • Real-time data • High frequency sampling • Continuous monitoring • Lower-cost method University of Wisconsin – Eau Claire

  3. Potential Benefits • Real-time data: • Simplify synoptic surveys • No need to return to lab to see results • Make quick decisions about further sampling • High frequency sampling • Currently possible but challenging • Required to characterize storm flows, mass fluxes (e.g., Balcom et al., 2004; Balogh et al. 1997; Mason et al., 1999) • Can provide resolution of individual rain events • May allow monitoring of new processes (e.g. throughfall) (e.g. Fisher & Wolfe, 2012) Balogh et al., 1997

  4. Potential Benefits • Continuous monitoring • Much less expensive • Can offer real-time data access via web • Less handling = more consistent data quality • Lower cost method • Enables more monitoring

  5. Approach • Design a system that: • Operates reagent-free • Uses minimal carrier gas • Requires maintenance < monthly • Is highly sensitive (0.1 ng/L detection limit) • Has high throughput (5 mins/sample) • Is self-cleaning (no carryover) • Is self-calibrating (no drift) • Is remotely controllable • Offers remote data access

  6. Simple Schematic

  7. Detailed Schematic Carrier Gas Inlet Calibrator Sample Loop Cleanup Trap Air Inlet Analytical Trap Catalyst Dryer Carbon Traps Pump Detector Filter Fan Decomp. Chamber Waste Temperature Controlled Zones Sample Inlet

  8. Instrument Overview Sample dryer and gold trap Sample decomposition chamber & catalyst Detector and calibration system Sample loop injection system Pinch valves Sample loop bypass Sample loop In Out Peristaltic pump

  9. Sample and Catalyst Chamber

  10. Gold Trap and Dryer

  11. Detector and Calibration System Loop 1 Loop 2 Carbon Trap Detector

  12. Enclosure

  13. Field Testing ¼” FEP Sampling Line

  14. Field Testing Ar Cylinder 0.45 µm Capsule Filter

  15. Results iPhone 4 Internet Explorer 10

  16. Results iPhone 4 Internet Explorer 10

  17. Instrument Control iPhone 4 Internet Explorer 10

  18. Software Overview User-customizable sequences

  19. Results • Linear calibrations over the course of the day • Temperature stability will minimize drift

  20. Results • Field testing data • Good retention time consistency • Optimizing to minimize carryover

  21. Goals for Finished Product • 0.1 ng/L detection limit • 5 mins/sample • < 0.1% carryover • Unattended operation for 1 month • Possible at current gas consumption with a size 40 cylinder (6.73” OD x 17.4” tall, 23.5 lbs.) • Reduce size and weight • Operate on standard 15 A, 120 V power outlet or lesspower

  22. Goals for Finished Product • Minimal signal drift over time • Robust performance with matrix interferences: • DOC • Dissolved solids • Extreme pH • Instrument control & data access via web portal and cellular/satellite data networks • Time-programmed or externally triggered sample analysis

  23. Development Schedule • February – November, 2012 • Phase I prototype development & testing • May – December, 2013 • Phase II re-engineering & lab testing • January – April, 2014 • Local field testing & design refinement • May, 2014 – January, 2015 • Beta unit production & field testing • February – April, 2015 • Finalize design & begin production

  24. Field Testing Locations King County USGS MDN ORNL EPRI

  25. What are your needs? • Software requirements • Hardware requirements • Sampling frequency • Detection limits • Portability • Power • Service frequency

  26. Acknowledgements • Steve Gunther, Brooks Rand • Phase I mechanical/design engineer • Paul Danilchik, Independent Contractor • Phase I electrical/software engineer • Carrie Miller, Oak Ridge National Lab • Phase I field testing partner • Jeremy Divis, Brooks Rand • Commercialization specialist • Colin Davies, Brooks Rand • President, project strategist • Department of Energy Small Business Innovation Research Program • Funding agency

  27. Questions?

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