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Collaborators
Collaborators
Clean Water
Clean Water
Clean Water
Clean Water
Advantages of nanomaterials for heavy metal separations
Advantages of nanomaterials for heavy metal separations
Examples of self-assembly in Nature
Examples of self-assembly in Nature
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Similar self-assembly forces contribute to micelle formation
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramic Substrates
Nanoporous Ceramics Substrate
Nanoporous Ceramics Substrate
Nanoporous Ceramics Substrate
Nanoporous Ceramics Substrate
So the way that we get the surface chemistry we need is…
So the way that we get the surface chemistry we need is…
So the way that we get the surface chemistry we need is…
So the way that we get the surface chemistry we need is…
So the way that we get the surface chemistry we need is…
So the way that we get the surface chemistry we need is…
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM: Self-Assembled Monolayers on Mesoporous Supports
SAMMSTM in a Nutshell
SAMMSTM in a Nutshell
Global Mercury Emissions
Global Mercury Emissions
Global Mercury Emissions
Global Mercury Emissions
Thiol-SAMMS™ overview
Thiol-SAMMS™ overview
Thiol-SAMMS™ overview
Thiol-SAMMS™ overview
TCLP Data for Hg-loaded thiol-SAMMS
TCLP Data for Hg-loaded thiol-SAMMS
Actual Hg waste clean-up
Actual Hg waste clean-up
The well had been treated using carbon type adsorbents to remediate
The well had been treated using carbon type adsorbents to remediate
Case Study 1: Results of 10 gpm Field Test on Well Water
Case Study 1: Results of 10 gpm Field Test on Well Water
Case Study 2: 10 gpm Field Test on Well Water with High Concentration
Case Study 2: 10 gpm Field Test on Well Water with High Concentration
Arsenic in Drinking Water Supplies
Arsenic in Drinking Water Supplies
Arsenic in Drinking Water Supplies
Arsenic in Drinking Water Supplies
The Anion Problem
The Anion Problem
Cu-EDA SAMMS Mechanism
Cu-EDA SAMMS Mechanism
Tailoring SAMMS™ to bind cesium
Tailoring SAMMS™ to bind cesium
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Tailoring SAMMSTM interfacial chemistry to the periodic table
Commercializing SAMMS
Commercializing SAMMS
Commercializing SAMMS
Commercializing SAMMS
Steward Environmental Solutions
Steward Environmental Solutions
Steward Environmental Solutions
Steward Environmental Solutions
Perry Equipment Corp
Perry Equipment Corp
Perry Equipment Corp
Perry Equipment Corp
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
SAMMSTM – Current Applications
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
Functional nanomaterials enhance analytical sensitivity/selectivity
SAMMS enhances electrochemical detection of heavy metals
SAMMS enhances electrochemical detection of heavy metals
SAMMS enhances electrochemical detection of heavy metals
SAMMS enhances electrochemical detection of heavy metals
Summary
Summary
Mercury Emissions
Mercury Emissions
10 gpm unit
10 gpm unit
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1Removing Heavy Metals from Water: 25SAMMS reduced [Hg] from input 4.5 ppt to
Self-Assembled Monolayers on Mesoporous 0.7 ppt within 6 minutes. Results provided
Supports (SAMMS). Glen E. Fryxell and by Steward Environmental Solutions.
Richard Skaggs March 11, 2008 WA Dept. 26Overview of different flavors of SAMMS
Ecology Olympia, WA Funded by DOE chemistry.
glen.fryxell@pnl.gov. Highlight article 27Arsenic in Drinking Water Supplies.
JMC 2007. Arsenic contamination of drinking water is
2Collaborators. Xiangdong Feng and Jun commonly natural, due to the local
Liu (early thiol SAMMS) Shas Mattigod, geology. US-EPA has a new drinking water
Yuehe Lin, Hong Wu, Sandy Fiskum, Kent standard as of Jan. 1, 2006 (down to 10
Parker, Wassana Yantasee (SAMMS testing) ppb from 50 ppb).
Ken Kemner and Shelly Kelly (EXAFS at ANL) 28The Anion Problem. Existing anion
Kenneth Raymond and Jide Xu (UC-Berkeley, exchange resins are generally based on
HOPO ligands) Tom Zemanian, Oleksiy quaternary ammonium salts and don’t allow
Ustyugov, Leo Fifield, Rose Galhotra (SCF) for direct interaction between ion pair
Shane Addleman, Tim Bays, Shari Li and Need a stereoselective receptor to bind
Brad Busche (analytical) Jerry Birnbaum, tetrahedral oxoanions. Chemistry of
Rob Wiacek (ligand synthesis) Theresa Materials 1999, 11, 2148-2154.
Hauser, Richard Champion (materials 29Cu-EDA SAMMS Mechanism. Kd’s for
synthesis and testing) Richard Skaggs chromate are very high (commonly 100,000)
(business development), Jim Toth (crude Kd’s for arsenate are moderately high
oil). (commonly 5,000-10,000) Kinetics are fast
3Clean Water. Clean-up technologies (minutes) While sulfate does compete, it
must address a wide variety of targets and is readily displaced. Journal of Physical
needs. Water quality, and access to clean Chemistry B, 2001, 105, 6337-6346.
drinking water, is emerging as one of the Chemistry of Materials 1999, 11,
global issues of the 21st century. 2148-2154.
4Advantages of nanomaterials for heavy 30Tailoring SAMMS™ to bind cesium.
metal separations. Nanomaterials provide: Anchoring an anionic ferrocyanide complex
High surface area (capacity) Well defined inside the pores of MCM-41 makes a very
structure High reactivity Readily tailored efficient cesium sorbent, even in the
for application in different environments, presence of large excesses of Na or K.
applications. Not all nanomaterials are Env. Sci. & Tech. 2001, 35, 3962-3966.
nanoparticles! 31Cesium SAMMS™ Summary. Kd’s for Cs
5Self-assembly is the spontaneous, binding are >100,000, even in the
ordered, organized assembly of molecules presence of 3M Na or K Excellent
(or particles), driven by a favorable selectivity – [Na] is more than 100,000
interaction with an interface and between times higher than [Cs] and yet 99.8+% of
the components. What is self-assembly? the Cs is still sequestered Good kinetics
6Examples of self-assembly in Nature. (minutes) Can strip Cs and regenerate the
Micelles and vesicles Cell membranes DNA sorbent activity via oxidation/reduction
?-helix Protein folding. of the Fe center.
7A brief history of synthetic 32Ligand Design Strategy for Actinide
self-assembly. Agnes Pockels, first SAMMS. Protic ligand -- a “hard” anionic
monolayers on the air-water interface Lewis base (e.g. carboxylate, phosphonate,
(1890s) Langmuir (air-water interface) etc.) Synergistic ligand -- amide carbonyl
films (1917) Blodgett (long chain fatty or phosphine oxide Synthesize a silane
acids on solids) (1930s) Interest in molecule containing both the desired
monolayer chemistry was rekindled in the protic and synergistic ligands in a
1980s: Sagiv, Whitesides, Ulman, Nuzzo, geometry suitable for chelation (CMPO
Alara, et al. (thiols on gold, and silanes analog) Proximity effects in the monolayer
on oxides) Explosion of activity in the interface will allow multiple ligands to
1990s (ribbons, tapes, sheets, etc.). interact with the actinide cation.
Excellent reference: “An Introduction to Environmental Science & Technology
Ultrathin Organic Thin Films: From 2005, 39, 1324-1331.
Langmuir-Blodgett to Self-Assembly” by A. 33Actinide-specific ligand synthesis.
Ulman; Academic Press; 1991. Hydrogen bonding between amide N-H’s helps
8Similar self-assembly forces to drive self-assembly. Ligand proximity
contribute to micelle formation. allows for multiple metal-ligand
Surfactant-Oil-Water Phase Diagram. interactions.
9Nanoporous Ceramic Substrates. 34Summary of Actinide SAMMS Studies.
Sol-gel. Surfactants R-N+-(CH3)3X-. Kd’s are pH dependant and typically
Template removal. 10,000-100,000 Excellent selectivity is
10Nanoporous Ceramics Substrate. ~5 – 10 possible Phosphonate esters show a
grams. “Bigger on the inside than it is on dependance on nitrate No competition from
the outside.”. Controlled pore channels: common cations (e.g. Na, Ca, etc.)
1.5 - 40 nm. Large surface area: ~600 - Phosphonic acids show no competition from
1000 m2/g. transition metals or complexants Excellent
11So the way that we get the surface sorption kinetics (minutes) HOPO ligands
chemistry we need is…. Molecular provide excellent actinide affinity, even
self-assembly. Self-assembly driven by Van for Np(V). Environmental Science &
der Waals interactions between chains, as Technology 2005, 39, 1324-1331.
well as the interaction between the Environmental Science & Technology
headgroup and the surface. Monolayer 2005, 39, 1332-1337.
Advantages Well-established silanation 35Tailoring SAMMSTM interfacial
chemistry Stabilized surface High ligand chemistry to the periodic table. ….all by
density Easily tunable chemistry. varying the monolayer ligand field.
“Designing Surface Chemistry in Mesoporous Cu-EDA. Thiol. Cu-FC-EDA. Cs. HOPO
Silica” in “Adsorption on Silica Prop-Phos. Env. Sci. & Tech. 2001, 35,
Surfaces”; pp. 665-687, Marcel-Dekker, 3962-3966. Chemistry of Materials 1999,
2000. Pore Surface. 11, 2148-2154 J. Physical. Chem. B. 2001,
12SAMMSTM: Self-Assembled Monolayers on 105, 6337-6346. J. Synchrotron Radiation,
Mesoporous Supports. +. 2001, 8, 922-924. Radiochimica Act 2003,
http://samms.pnl.gov/. First reported in: 91, 539-545. Env. Sci. & Tech. 2005,
Science 1997, 276, 923-926. A. 39, 1324-1331 . Env. Sci. & Tech.
Self-assembled monolayers. B. Ordered 2005, 39, 1332-1337 . J. Materials
mesoporous oxide. Chemistry 2004, 14, 3356-3363 Chem. Comm.
13SAMMSTM in a Nutshell. Extremely high 2002, 1374-1375. Science, 1997, 276,
surface area = high binding capacity 923-926. J. Synchrotron Radiation, 1999,
Rigid, open pore structure provides for 6, 633-635 Sep. Sci. & Technol. 1999,
fast sorption kinetics Chemical 3411, 2329-2345 Mat. Tech. Adv. Perf. Mat.
specificity dictated by nanopore 1999, 14, 183-193 Surf. Sci. &
interface, easily modified for new target Catalysis, 2000, 105, 729-738.
species Proximity effects can allow 36Life-cycle considerations. What
multiple ligand/cation interactions happens after the heavy metals are
Particle size generally on the order of captured? Direct disposal Hg laden SAMMS
50-100 micron (but can be tailored either passes TCLP leachate test Landfill,
larger or smaller) Engineered forms hazardous waste (minimal volume) Treatment
(canisters, cartridges, membranes, etc.) followed by disposal Grouting Cement
Regenerable. “Environmental and Sensing monolith Vitrification (only viable for
Applications of Molecular Self-Assembly” certain heavy metals) Strip the toxic
in “Encyclopedia of Nanoscience and metal and recycle SAMMS™ Regeneration has
Nanotechnology”; Dekker, 2004, pp. been demonstrated Recycling holds down
1135-1145. materials costs, but increases labor costs
14Global Mercury Emissions. Recent and potential worker exposure.
estimates of total global mercury 37Commercializing SAMMS. Teaming with
emissions (per year) from all sources are private industry to make high performance
roughly 6,000 metric tons emitted per year sorbents for heavy metal removal. TM. A
(range from 4,400 to 7,500). These Path Forward.
emissions are split into 3 roughly equal 38Steward Environmental Solutions.
parts: Source: United Nations Environment Carrier bead powders, iron silicides,
Programme Global Mercury Assessment, 2002, ferrites, custom ceramic design and
using J. Pacyna 1995 data, as presented by processing Based in Chattanooga, Tennessee
the Arctic Monitoring and Assessment Well connected in the power industry (coal
Programme and nuclear) Has licensed the SAMMS
http://www.epa.gov/mercury/control_emissio patents, including SCF methodology
s/global.htm. Currently targeting Hg capture in
15Thiol-SAMMS™ overview. Thiols have coal-fired power plant emissions. SES
high affinity for “soft” heavy metals contacts: Bob Jones --
(e.g. Hg, Cd, Au, etc.). High Kd values rjones@stewardsolutions.com John Higley --
for Hg binding (e.g. 10,000,000). No jhigley@stewardsolutions.com. Ferrite
competition from common ions (e.g. Na, Ca, powders.
Fe, etc.). Thiol SAMMS™ even out-competes 39Perry Equipment Corp. A leading player
a variety of complexants. High saturation in industrial filtration (oil/gas,
binding capacity (as much as 2/3 of its chemical, food/beverage, etc.) Based in
own weight in Hg, depending on Mineral Wells, Texas (with facilities in
conditions). Journal of Materials US, Canada, Mexico, Europe, Middle East,
Chemistry 2007, 17, 2863 – 2874. Asia). Purchased by Clarcor Corp in 2007.
Mercaptopropyl siloxane monolayer lining Aggressively interested in incorporating
the pore surface of mesoporous silica. The nanotechnology (SAMMS) into filtration
mercury (shown in blue) binds to the technology Filter elements, vessels,
sulfur atoms (sulfur atoms are shown in engineering services Currently targeting
yellow). Hg removal from produced water in the
16Mercury Adsorption Kinetics: Thiol petroleum industry. Industrial filtration
SAMMS™. GT-73. SAMMS. elements.
17TCLP Data for Hg-loaded thiol-SAMMS. 40SAMMSTM – Current Applications. Flue
18Actual Hg waste clean-up. Case #1. Gas. Produced Water. Mining impoundments.
Case #2. Case #3. 10L of lab waste (146 Sensors. Coal gasification.
ppm Hg) Est. disposal cost $2000 86 g of 41Functional nanomaterials can make
Thiol SAMMS used (final Hg conc. 0.04 ppm) analytical tools faster, more sensitive.
Treatment cost $180 10-fold reduction in High surface areas Open pore structure
cost. 200L of EVS scrubber waste (4.64 ppm High functional density Easily tailored to
Hg) Est. disposal cost $3400 Thiol SAMMS conform to analytical interface. Ceramic
used (final Hg conc. 0.05 ppm) Est. nanosorbents Highly versatile silane
treatment cost $210 15-fold reduction in chemistry Easily templated, processed.
cost. Mixed waste oils (0.8-50 ppm Hg) E-chem. XRF. High-performance
Thiol SAMMS used (final Hg conc. <0.2 preconcentrators. UV-Vis. GC. IR.
ppm) Only method proven effective in Radiocounting.
hydrophobic media. Ref: Klasson et al. 42Functional nanomaterials enhance
1999, 2000 ORNL. analytical sensitivity/selectivity.
19INL/SES demonstration/deployment. High-performance pre-concentrators.
Idaho National Laboratory V-9 Wastes Sensor. Electrochemical sensors.
Complex slurry of aqueous, heavy metals, Nanoparticles. Nanopores. Radiochemical
radionuclides (e.g. Cs-137, Co-60, assay. Nanorods. Spectroscopic detection.
Eu-152), solids, halogenated solvents Functional nanomaterial interface.
(TCE, TCA, PCE, etc.), etc. Hg 43SAMMS enhances electrochemical
concentration 1.57%, speciation unknown detection of heavy metals. Lead.
(mixed?) Planning to solidify the waste Environmental Health Perspectives, 2007,
using Waterworks SP-400 (10% by weight). 115, 1683–1690. PNNL sensor uses SAMMS:
Problem: Hg still leachable Viable Incorporate high surface area, chemically
strategy in place for the other hazards, specific sorbent material into working
needed the ability to immobilize the Hg in electrode Sorbent can be tailored for
situ such that the final wasteform would different target analytes - Small
pass TCLP. Tests showed that Thiol-SAMMS™ headspace size and variable flow volumes
could effectively immobilize the Hg in allow sample size to be varied over wide
place and that the resultant wasteform ranges. First level of discrimination
could pass TCLP by an order of magnitude. provided by the chemical selectivity of
Successfully treated the entire contents the SAMMS Second level of discrimination
of tank V-9 with thiol-SAMMS. provided by the electrochemical response
20The well had been treated using carbon of the analyte during stripping voltametry
type adsorbents to remediate mercury but Ppb sensitivity with multiple metals (Pb,
was experiencing frequent adsorbent Cd, Cu, etc.) Response is linear to
fouling problems and was unable to meet concentration Efficient preconcentration
potential future low mercury reduction Works in environmental water samples,
targets ? 12 ppt output. The well water blood, urine, etc. Lunch-box sized field
contained over twenty inorganic species. test system.
Steward’s conducted bench testing (batch) 44Summary. SAMMS™ is a very effective
and demonstrated SAMMS® was able to reduce method for separation and sequestration of
[Hg] from input ~25 ppb down to ~14 ppt. environmentally problematic species Rapid
Steward conducted a field test using 10 sorption kinetics and high binding
gpm SAMMS filtration system with four capacity SAMMS can be readily tailored for
contactor tanks. Case Study 1: Well Water a variety of environmental target species
Remediation Field Test. Chemistry can be tailored to capture heavy
21Case Study 1: Results of 10 gpm Field metals, oxometallate anions, actinides,
Test on Well Water. Field test ran 1,300 cesium, etc. SAMMS are now being made
hours and processed over 450,000 gallons commercially by Steward Environmental
of well water. SAMMS reduced [Hg] from Solutions Same chemistry can be used to
input ~25 ppb down to below detection enhance sensing technologies. Available at
limits (EPA 245.7) at output (~ 5ppt), amazon.com.
well below 12 ppt mercury reduction goal. 45
Field test verified the high mercury 46Extra slides.
adsorption capacity of SAMMS (~ 40 pounds 47Mercury Emissions. EPA’s Clean Air
of SAMMS used). Mercury laden SAMMS from Mercury Rule (CAMR) (3/15/05) Current
the field test was tested and passed TCLP. estimated US power plant emissions are
Results provided by Steward Environmental about 48 tons Hg/year (158 tons
Solutions. anthropogenic Hg/year total). Current air
22Case Study 2: 10 gpm Field Test on pollution control devices can capture some
Well Water with High Concentration of Hg, but this varies widely depending on a
Dissolved Solids: Well water was very dark number of variables Current baseline
brown in color (humic acid) and contained estimates: $50,000-$70,000 per pound Hg
high concentrations of total dissolved removed ($4.3B to $6.7B) Near-term goal:
solids and organics. Activated carbon 50-70% Hg capture, at 25-50% reduction in
failed repeated tests due to fouling. The cost (2010) Longer-term goal: 90+% capture
water contained more than twenty known (2018). We are currently developing new
species, such as sulfide, iron and classes of SAMMS (and related materials),
chlorobenzene. A batch bench with SAMMS specifically tailored for application to
demonstrated reduction [Hg] to meet an high temperature, vapor phase applications
initial target of 90% reduction. A field (IGCC and CTL).
test was conducted using a 10 gpm SAMMS 48Electrochemical detection system. Uses
contactor tank system and ozone magnetic nanomaterials to enhance
pretreatment to reduce organics. analytical speed/sensitivity Cheap,
23Case Study 2: 10 gpm Field Test on lunchbox sized Field portable Measures
Well Water with High Concentration of heavy metal content of aqueous samples,
Dissolved Solids: SAMMS reduced [Hg] in blood, urine and saliva ppb sensitivity
over 40,000 gallons of well water from for multiple metals in 3-4 minutes.
input ~2,000 ppt down to ~ 10 ppt output, Environmental Health Perspectives, 2007,
well below 90% mercury reduction goal. 115, 1683–1690.
Mercury laden SAMMS from the field test 4910 gpm unit. Photo provided by Steward
was tested and passed TCLP. Results Environmental Solutions.
provided by Steward Environmental 50Run this through ERICA. We will make
Solutions. an at large request for a test site for
24Case Study 3: SAMMS for Mercury soils clean up using SAMMS Bring
Reduction to Ultra Low Concentration: An touchy-feelies (SAMMS, extrudates, PECO
existing water treatment system, could not filter cartridge, also bring slides with
reach the mercury reduction target of 1.3 pictures of SES test-bed apparatus) Bring
ppt or lower and SAMMS was tested as an presentation on thumb-drive (can also
alternative. 2. A SAMMS batch bench test email it ahead to Maria) Audience will be
was performed. very concerned with end of life issues and
25Case Study 3: SAMMS for Mercury life-cycle issues (disposal).
Reduction to Ultra Low Concentration:
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