emulsified zero-valent iron laboratory and field testing · emulsified zero-valent iron laboratory...
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EMULSIFIED ZERO-VALENT IRON Laboratory and Field Testing
Jacqueline Quinn, Ph.D.
NASA Kennedy Space Center
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Research Participants
• Chris Clausen and Cherie Geiger from University of Central Florida
• Suzanne O’Hara, Tom Krug and Dave Major from GeoSyntec
• Tom Holdsworth from USEPA NRMRL • Bob Puls and Chunming Su from USEPA
GWERD• Nancy Ruiz from NFESC Navy
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Technology Rationale
• ZVI PRBs are effective in treating dissolved CVOCs but:
• are dependent on dissolution and transport of CVOCs; and • do little to reduce the clean up time and long-term monitoring
costs.• ZVI needs to be in the presence of water to promote reductive
dehalogenation injection of ZVI into a DNAPL source zone will only treat the dissolved phase at the edges of the DNAPL.
• EZVI can be used to enhance degradation of DNAPLs by enhancing contact between the DNAPL and the ZVI particles.
DNAPLSource
Area
Dissolved CVOC
ZVI PRB
Treated Water
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• Emulsion droplets contain iron particles in water surrounded by an oil-liquid membrane
• EZVI composed of food-grade surfactant, biodegradable vegetable oil, water, and ZVI (nano- or micro-scale iron)
WaterOil
SurfactantIron
Properties of EZVI
12. 3 μm
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DNAPLdyed red
DNAPL with micro-scale ZVI
DNAPL with EZVI
EZVI In Contact with DNAPL
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• Demonstration conducted at NASA’s LC34.
• Performance evaluation based on GW mass flux and TCE mass in pre- and post-treatment soil cores
•Monitored changes in CVOCs in:
• GW (5 depth intervals, 2 upgradient and 2 downgradient wells); and • soil cores (8 depth intervals, 6 locations)
• EPA SITE Program independently evaluated technology demonstration
EZVI Technology EvaluationDemonstration at LC34
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Field Demo EPA SITE Program Report
• Battelle conducted an independent evaluation of the EZVI demonstration at LC34
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Field Demo Paper in ES&T
• ES&T published special issue on nanotechnology
• NASA and GeoSyntec co-authored paper in this issue on the EZVI Field Demonstration
• Quinn et al. 2005 Field Demonstration of DNAPL Dehalogenation Using Emulsified Zero-Valent Iron. Environ. Sci. Technol. 2005, 39, 1309-1318.
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Results of Demo at LC34Soil Core Samples:
• Stated objective of 50% removal of total TCE
• EZVI migrated to shallow intervals with PPT injection
• Significant reduction of TCE in four months (>80%) where EZVI was present
• Average reduction of 58%EZVI in 1- to 3-inch thick stringer
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Results of Demo at LC34
• Groundwater Samples:
• Significant reduction (60 to 100%) of TCE in target depths.
• Reduction of 56% in the Mass Flux.
• Elevated cis-1,2-DCE, VC suggest biodegradation due to oil as an electron donor may also be significant
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Recommendations From LC34 Demonstration
• Promising results at LC34 but needed to further evaluate:
– how to control placement of EZVI in subsurface
– the contribution of the abiotic and biological components of the degradation
• ESTCP funding acquired to address these questions
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ESTCP-funded Treatability Testing• Lab tests conducted to evaluate treatment of near saturation
dissolved phase concentrations (1000 ppm) and DNAPL (10 x saturation) using:– Controls (active and sterile)– Vegetable oil & surfactant (Emulsion)– Nano-scale zero-valent iron (nZVI)– Emulsified zero-valent iron (EZVI)
• Monitor VOCs, DHG and Chloride
• Treatability tests done in triplicate andeach test set up is done in both sterile and non-sterilized set ups
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Dissolved Phase Treatments• Near saturation concentrations of TCE
• TCE of 1,000 mg/L (0.8 mmoles per bottle)
• nZVI added to achieve 5 times theoretical ZVI requirement to degrade TCE
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• No losses of TCE or production of degradation byproducts observed in control treatments
Active Control
• TCE concentration drops to 0.1 mmols- sequestered in oil
• No degradation by-products observed until ~day 50 when pH buffered and re-bioaugment with KB-1
• Impacts of biodegradation not significant in these tests which utilized DI water and no soil
Oil Emulsion Treatment
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TCE cis-1,2-DCE VC Ethene Ethane
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TCE cis-1,2-DCE VC Ethene Ethane
Dissolved Phase Testing (1)
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nZVI Treatment• TCE concentrations drops
very rapidly • Undergoes rapid and
complete degradation• TCE is non-detect by day 71
EZVI Treatment• TCE concentration drops very
rapidly • EZVI treatment undergoes
slightly slower degradation but also complete degradation
• TCE is non-detect by day770
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TCE cis-1,2-DCE VC Ethene Ethane
Dissolved Phase Testing (2)
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Chloride Production with Dissolved TCE
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ZVI EZVI Oil Control
100% conversionof TCE toethene
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Conclusions - Dissolved Phase Testing• Dissolved Phase Testing:
– Lab tests show that EZVI degradation, especially at early times, is mainly due to ZVI (abiotic)
– Abiotic degradation of the ZVI in the EZVI is not adversely impacted by the oil
• So why use the EZVI if the nZVI promotes rapid and complete degradation?
• In the presence of dissolved phase the ZVI may be slightly faster but in the presence of DNAPL the advantages of the EZVI become apparent
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DNAPL Phase Treatments• 10x saturation concentrations of TCE
• TCE of 10,000 mg/L (16.7 mmoles per bottle)
• nZVI added to achieve 2 times theoretical ZVI requirement to degrade TCE
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Active Control
• TCE at saturation concentration
• No degradation by-products observed (no DHG or chloride)
• TCE stable at ~30% of saturation concentration
• No degradation by-products observed (no DHG or chloride)
• DNAPL sequestered in oil phase –equilibrium concentrations lower than for pure phase DNAPL
Oil Emulsion Treatment
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TCE cis-1,2-DCE VC Ethene Ethane
DNAPL Testing (1)
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nZVI Treatment• TCE stable at saturation
concentration• Degradation by-products
observed (ethane and ethene)
• Chloride production indicates degradation of ~73% of TCE
EZVI Treatment• TCE ~10% of saturation
concentration and dropping• Degradation by-products observed
(ethane and ethene)• Chloride production indicates
degradation of ~71% of TCE
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TCE cis-1,2-DCE VC Ethene Ethane
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TCE cis-1,2-DCE VC Ethene Ethane
DNAPL Testing (2)
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ZVI EZVI Oil Control
70% conversionof TCE toethene
Chloride Production with DNAPL
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Conclusions of DNAPL Testing• Veg Oil Emulsion decreases TCE concentration due to
sequestration (no degradation)
• nZVI reduces mass of TCE due to treatment but no decrease in aqueous concentration of TCE (no effect on mass flux)
• EZVI benefits from sequestration due to oil plus degradation due to nZVI
– Significant decrease in aqueous concentrations (drop in mass flux) greater then with just the oil; and
– Reduction in mass of TCE
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• Former dry cleaner site
• Buildings have been torn down
• Source areas located around former above and below ground storage tanks
• Evaluate two injection methods and performance assessment of EZVI’s ability to degrade VOCs
Demonstration SiteParris Island MCRD, SC
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Technical ProgressDNAPL Distribution and Well Installation
• 9 soil cores and groundwater samples collected in 2005 and 2006 to evaluate contaminant distribution
• Wells installed in July 2006 to target the source areas identified through cores
• EPA (GWERD, National Risk Management Research Laboratory) provided drill rig for coring and well installation
SC-9
Previous Storage Tank Area Direct Injection Plot
Pneumatic Injection Plot
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Technical ProgressDNAPL Distribution and Well Installation
Pneumatic Injection Plot
Direct Injection Plot
Multilevel Well Construction Direct & Pneumatic Injection Plots
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sand
silty clay
sand
peat
0 ft
5 ft
10 ft
15 ft
20 ft
Pneumatic Injection PlotDirect Injection Plot
sand
silty sand
sand
peat
sand/clay
Technical ProgressDNAPL Distribution and Well Installation
Fully screened and multilevel wells
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Baseline Characterization
Groundwater Sampling• Groundwater sampling and analysis
support provided by EPA• EPA personnel participate in all
groundwater sampling events and some groundwater samples analyzed at Kerr Laboratories, Ada, OK
• Baseline samples collected from over 50 sample locations (including multilevel wells) during June, August and October 2006 sampling events (2-week sampling events)
• Sample parameters include field parameters (DO, ORP, pH, temperature, conductivity, turbidity) VOCs, DHGs, VFAs, anions, alkalinity, TOC/TIC, metals (dissolved, total), and isotopes (O, H, Cl)
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Baseline Characterization
Groundwater Sampling• DNAPL pumped out of ML-2-5 up-gradient of
plot
• Multilevel wells: changes in groundwater mass flux downgradient of plot and evaluate incoming flux to plot (located within a larger plume)
• Fully screened wells: integrated samples within plot for performance evaluation and external to plot to evaluate changes during injection of EZVI
DNAPL
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EZVI Preparation
• EZVI made on-site by combining:• Nano-scale iron (Toda)• Corn oil
• Ingredients added to drum and mixed using a top mounted industrial mixer
• EZVI pumped from mixing drums into injection tanks
• Surfactant• Water
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EZVI Injection
Pneumatic Injection Plot• Total of 575 gal EZVI injected into 8 locations within the Pneumatic
Injection Plot between 7 and 19 ft bgs (2 locations using Direct Injection)
• During injections, monitored injection pressure, pressure distribution in subsurface, ground heave, and looked for EZVI at ground surface
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0 5 10Feet
0 5 10Feet
EZVI Injection
Pneumatic Injection Plot• Total of 575 gal EZVI injected into
8 locations within plot between 7 and 19 ft bgs (2 locations using Direct Injection)
• During injections, monitored injection pressure, pressure distribution in subsurface, ground heave, and looked for EZVI at ground surface (shown as grey areas on figure)
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EZVI Injection
Direct Injection Plot• Total of 150 gal EZVI injected into
4 locations within plot between 6 and 12 ft bgs
• During injections, monitored injection pressure and looked for EZVI at ground surface
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0 5 10Feet
0 5 10Feet
EZVI Injection
Direct Injection• Total of 150 gal EZVI injected into
4 locations within plot between 6 and 12 ft bgs
• During injections, monitored injection pressure and looked for EZVI at ground surface
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EZVI Injection
• EZVI observed at ground surface in both Pneumatic Injection and Direct Injection Plots
Pneumatic Injection plot (daylighting around ML-3 pad,
down-gradient of plot)
Direct Injection plot (daylighting possibly from
old soil core location)
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EZVI Injection
EZVI Soil Cores• Collected cores to evaluate
ability of injection technologies to distribute EZVI evenly over the target treatment intervals
sand saturated with EZVI
• Possible EZVI in all soil cores except ESC-06
ESC-04, 12-16ft
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Performance MonitoringBaseline Samples
June 2005, June, August & October 2006
November 2006
January 2007
March 2007
Field Parameters 71 27 32 27 157VOCs 136 27 32 27 222DHGs 114 27 32 27 200VFAs 23 19 4 23 69Anions 71 27 32 27 157Alkalinity 71 27 32 27 157TOC/TIC 71 27 32 27 157Metals (dissolved) 71 27 32 27 157Metals (total) 71 27 32 27 157Isotopes (Cl) 6 - - 6 12Isotopes (O, H) 6 6 6 6 24VOCs 70 - - - 70EZVI cores (4ft) 32 - - - 32foc, porosity 3 - - - 3
**Sample numbers do not include additional 10% QA/QC samples
Total Samples To Date
GR
OU
ND
WA
TER
SOIL
Parameter Performance Monitoring Samples
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Performance MonitoringGroundwater Sampling Summary
• In general, downgradient wells show decrease in PCE/TCE with increase in degradation products including significant increases in ethene
• Upgradient wells and PMW-5 show continued presence of DNAPL although significant production of ethene in PMW-5 indicates that degradation is ongoing in the area
• Significant increases in VFAs (primarily acetic and propionic acids) and TOC
• Small decrease in pH, and increases in iron (dissolved and total)
• DNAPL now being pumped from ML-2-7 and PMW-5 (inside Pneumatic Injection plot) and from PMW-4 (south [transgradient] of Pneumatic Injection plot) as well as from ML-2-5 where DNAPL was present pre-injection
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Performance Monitoring
ML-3-5ML-5-5 ML-5-5ML-7-5
ML-3-5
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Performance MonitoringPneumatic Injection
PMW-5 PMW-6
Interior Wells
PMW-3
Downgradient Well
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• Continued monitoring at Parris Island proposed through Oct 09
• Continued use throughout US
• One licensee getting ready for European deployment
• EZVI has taken one private client’s site off the NPL
Next Steps
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Questions?
EZVI team being inducted into the Space Technology Hall of Fame