2015

Issue 2

Science & Technology at the Ames Laboratory

w CUTTING-EDGE ANALYSIS

w BACKING A BIG IDEA

wSOLVING THE PLANT PUZZLE w CATALYSTS FOR CHANGE
Adam Schwartz, Director

Contents

Copyright 2015 by Ames Laboratory. All rights 

reserved. For additional information about Ames 

Laboratory or topics covered in this publication, 

please contact: 

ENERGY

U.S. DEPARTMENT OF Office of

Science Inquiry Issue 2 | 2015 3

From the Director

There’s Chemistry in Our Chemistry

hemistry, broadly defined, is the science of change. Chemists study matter 

to identify its components and determine the properties and ways in which those 

components interact, combine and change. They then use their understanding of 

those processes to form new substances.

Chemistry can also mean that special connection between two people or a group of people. 

Casting directors strive for that type of chemistry when pairing the leading actors for a motion 

picture or stage production. Sports fans look for a similar “spark” between a quarterback and 

his favorite receiver or a cagey point guard who can dish out a no-look pass to the big man for 

a thundering slam dunk.

As you’d expect, Ames Laboratory research involves a lot of the first type of chemistry and 

it’s the cornerstone of our Division of Chemical and Biological Sciences. As you’ll discover 

in the articles in this issue of Inquiry, our chemists are designing new catalysts to power 

chemical reactions without the need for powerful (and possibly toxic) solvents or large inputs 

of energy (see page 6). They’re also looking at the chemical processes in plants and developing nondestructive techniques to analyze plant material as it grows in hopes of more efficiently harnessing the energy in 

biomass (page10). 

Others are using state-of-the-art dynamic nuclear polarization (DNP) solid-state nuclear magnetic resonance 

(NMR) spectroscopy to take a look at molecular structures of materials at unprecedented resolution (page 13). 

There’s also a group studying the big idea of how to mine the energy that winds up in landfills, particularly in the 

form of plastics (page 16). One of the biggest hurdles is that the plastic is mixed in with other materials, requiring a 

strategy to chemically convert that mixed waste stream into something useable.

But there’s plenty of the second type of chemistry at the Ames Laboratory 

as well. From the beginning, Ames Laboratory has fostered a collaborative 

environment that brings together the synthesis, characterization and theoretical 

aspects of research projects. Experimentalists develop the materials, analytical 

researchers provide the necessary measurements and theorists model what’s 

occurring. The model in turn provides a suggested roadmap for additional 

experimentation and characterization.

Ames Laboratory also has great chemistry with its contractor, Iowa State 

University. As the only one of DOE’s 17 national laboratories physically 

located on a university campus, Ames Laboratory can leverage the resources – 

personnel, equipment and facilities – of Iowa State and vice versa. Nowhere is 

this chemistry more evident than the new Sensitive Instrument Facility that will 

formally open for operation in May 2016 (see page 5).

Through cooperative efforts, the SIF was equipped with cutting-edge electron microscopy equipment that will 

benefit both Ames Laboratory and Iowa State researchers. The final piece of equipment, a $3.5 million aberrationcorrected scanning transmission electron microscope, just arrived and will be installed in January. Everyone involved 

in the project is anxiously awaiting the boost this facility collectively provides us.

Lastly, there’s a wonderful rapport that’s created through our ongoing DOE-sponsored internship programs. 

Through the Science Undergraduate Laboratory Internships (SULI), Visiting Faculty Program (VFP) and Community 

College Internships (CCI) programs, students and faculty participate in research projects with Ames Laboratory 

scientist mentors. While the benefits to these students are obvious, our researchers also find the experiences 

rewarding (see page 18). 

Thanks and enjoy learning about the chemistry that makes Ames Laboratory what it is.

C

Inquiry is published biannually by the Ames 

Laboratory Office of Public Affairs. Iowa 

State University operates Ames Laboratory 

for the U.S. Department of Energy under 

contract DE AC02 07CH11358. 

Editor, Inquiry

Ames Laboratory

111 TASF

Ames, Iowa 50011-3020

515-294-9557

www.ameslab.gov

Ames Laboratory is a U.S. Department of Energy national laboratory seeking solutions to energy-related problems 

through the exploration of chemical, engineering, materials and mathematical sciences, and physics. Established 

in the 1940s with the successful development of the most efficient process to produce high-purity uranium metal 

for atomic energy, Ames Laboratory now pursues much broader priorities than the materials research that has 

given the Lab international credibility. Responding to issues of national concern, Ames Laboratory scientists are 

actively involved in innovative research, science education programs, the development of applied technologies 

and the quick transfer of such technologies to industry. Uniquely integrated within a university environment, the 

Lab stimulates creative thought and encourages scientific discovery, providing solutions to complex problems and 

educating and training tomorrow’s scientific talent.

Steve Karsjen: Public Affairs Director

Kerry Gibson: Editor

Breehan Gerleman Lucchesi: Contributing Editor

Laura Millsaps: Contributing Editor

Grant Luhmann: Art Director

From the beginning, Ames 

Laboratory has fostered a 

collaborative environment 

that brings together the 

synthesis, characterization 

and theoretical aspects of 

research projects. 

4Awards

5SIF

Nearly Operational

Ames Lab Scientists Strengthen Research Through Teamwork

10 Solving the Biomass Puzzle

6

P A G E Collaboration Equation: 

DNP in 2015 13 16

Waste Stream to Energy Source: 

Chemists Leave 

Their Mark on 

Future Scientists 

18
Awards

4 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 5

Fidler named LANL Director’s Fellow

The awards for research excellence just keep stacking up for Andrew Fidler, 

former Science Undergraduate Laboratory Internship (SULI) program intern at 

Ames Laboratory.

Fidler’s latest award comes from Los Alamos National Laboratory (LANL), 

the Department of Energy national laboratory where he’s currently serving as a 

postdoctoral fellow. Fidler was named one of LANL’s Director’s Fellows. Director’s 

Fellows collaborate with LANL scientists and engineers on staff-initiated research. 

Award selections are based on academic and research accomplishments and the 

strength and potential impact of the proposed research.

Outstanding Technical Paper 

Ames Laboratory graduate student 

Stephanie Choquette and scientist Iver 

Anderson received the 2015 Howard I. 

Sanderow Outstanding Technical Paper 

Award from the Metal Powder Industries 

Federation and its Technical Board.

T h i r t y - t w o p a p e r s f r o m t h e 

POWDERMET2015 conference, held 

in May in San Diego, were evaluated 

for final selection. Choquette and 

Anderson’s paper, “Liquid-Phase Diffusion 

Bonding: Temperature Effects and Solute 

Redistribution in High Temperature LeadFree Composite Solders,” was selected as 

the top paper from that group.

Andrew Fidler

Laboratory receives GreenBuy Silver Award 

Ames Laboratory recently met one of the 2014 Environmental Management 

System Steering Committee (EMSSC) goals by winning the DOE GreenBuy 

Program Silver Award for Sustainable Acquisitions. The Laboratory was one of 

four laboratories to earn an award from the GreenBuy Program. 

To achieve the Silver Award, sites must meet the recycled content or energy 

savings requirements for a minimum of six products in at least three product 

categories. In the construction category, Ames Laboratory met 100 percent of 

the requirements for carpet and flooring materials. Toilet tissue purchases met 

the requirements within the custodial category. Three of the four office category 

products purchased (binders, copy paper and servers) met 100 percent of the 

requirements, while 97 percent of office furniture met the goals of the program. 

Cassie Dewey, Sallie Spencer 

and Sarah Morris-Benevides with 

some of the products that helped 

Ames Lab earn the DOE Greenbuy Silver Award (center).

Ames Lab named FLC Outstanding Laboratory

Ames Laboratory was named Outstanding Laboratory by the Federal 

Laboratory Consortium for Technology Transfer Midwest Region. The award 

is presented to the management of a Mid-Continent member laboratory 

or facility that has provided exceptional support and encouragement to 

the transfer of federal technologies to the private sector. Such support and 

encouragement must have provided tangible benefit to the private sector and 

to the general public. 

Ames Laboratory’s Associate Director for Sponsored Research Debra 

Covey nominated the Lab for the award, based in large part on the work of 

the Critical Materials Institute.

Iver Anderson and Stephanie Choquette

Todd Zdorkowski (left) and Deb Covey present Ames Laboratory Director Adam 

Schwartz with the Federal Laboratory Consortium for Techology Transfer MidContinent Region Outstanding Laboratory Award. Zdorkowski received the 

award on behalf of the Laboratory at the FLC’s Mid-Continent Region annual 

meeting on Aug. 26. 

After more than a year of construction, Ames 

Laboratory’s new Sensitive Instrument Facility is close to 

being operational. The wet and dry preparation labs have 

been completed and state-of-the-art microscopy equipment 

has been installed. The focused-ion beam microscope is 

currently operational and other pieces are being calibrated 

and tested. A grand opening of the facility is being planned 

for May 2016.

Nearly Operational

Microscopy equipment began arriving in October. Here, the 

focused-ion beam microscope is carefully unloaded.

The building has sample preparation areas for both wet and 

dry samples, along with a separate instrument repair area.

The SIF lobby features seating outside the two offices for 

operational staff, shown in the background.

This transmission electron microscope was the lone piece of 

existing equipment that was transferred to the SIF.

The lobby is decorated with artwork showing microscopy images submitted as part of a competition.

The Sensitive Instrument Facility (SIF) is Ames Laboratory’s 

first new research building in 60 years. 
Theresa Windus

Igor Slowing

Collaboration Equation: 

Ames Lab Scientists Strengthen Research Through Teamwork

hese days, the fictional stereotype of the

isolated and misunderstood scientist toiling alone in 

his or her lab could not be further from the truth. 

With scientific disciplines both widely diversified 

and highly specific, it takes a team of researchers to integrate 

those disciplines into a unified research goal. 

At the Ames Laboratory’s Chemical and Biological 

Sciences Division, a team of scientists advance the frontiers 

of catalysis—the acceleration of chemical reactions—

through the use of three-dimensional nano-particles. 

The beginnings of the 3D catalysis project in 2002 was 

sparked by nuclear magnetic resonance spectroscopy expert 

Marek Pruski and the late Ames Laboratory scientist Victor 

Shang-Yi Lin. Together they wanted to pair the development 

of three-dimensional scaffolds for catalysis designed by 

Lin with the best possible NMR spectroscopy methods for 

characterizing them developed by Pruski. “It was a natural 

symbiotic relationship,” remembers Pruski.

And just like reactions are spoken of in the language of 

chemical equations, over time the interactions of scientists 

in the Ames Laboratory’s catalysis program have created an 

equation of their own, where the right balance of experiment, 

characterization and theory adds up to something more than 

the sum of their individual parts. 

Chemist2

“We’re creating fundamental and unique chemical 

functions for important transformations.” 

 

– Aaron Sadow

Ames Laboratory scientist Aaron Sadow studies chemical 

reactions that can be manipulated and controlled toward a 

specific purpose. With an interest in organometallics, he hunts 

for catalysts that can be stabilized and made more efficient 

for petrochemical, biorenewable, and shale-gas chemical 

processes. 

“We’re creating fundamental and unique chemical functions 

for important transformations,” said Sadow. 

He collaborates with scientist Igor Slowing, who specializes 

in developing mesoporous nanoparticles from silica and other 

materials that provide a platform for these chemical reactions 

to take place.

While the creation of new and useful catalysts is a goal, 

so is understanding specifically how these three-dimensional 

catalytic structures function the way they do. 

“When we attach these catalysts to materials, we’re changing 

how they perform. We’re comparing heterogeneous or nonsoluble forms to soluble forms of the catalyst, the effects of 

immobilizing them in these support systems, and how they 

work differently,” said Sadow. 

“We’re trying to understand how the structure and design 

of these platforms affect the catalytic processes,” said Slowing. 

T

Marek Pruski

Aaron Sadow

Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research w Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research w Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research

6 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 7

BY LAURA MILLSAPS
“The pores in these particles force molecules to move in 

different ways, and we need to know more about that in order 

to optimize these catalytic systems to work the most efficiently.”

NMR spectroscopy

“Honestly, without Marek we’d be flying 

blind.” 

 – Aaron Sadow

Marek Pruski’s group provides guidance to other project 

members with the structural insights. To do so, Pruski 

uses Ames Laboratory’s state-of-the-art solid-state NMR 

instrumentation, including the recently acquired dynamic 

nuclear polarization (DNP) NMR spectrometer, the first 

in the nation to be used exclusively for materials science 

research. Its use represents up to a 300-fold increase in 

sensitivity and a “transformational” technique in providing 

information to experimental researchers and theorists. 

“No other method of spectroscopy can probe the structure 

of materials with such atomic-level sensitivity to the local 

electronic environment,” said Pruski. “Until you carry out 

proper characterization of a catalyst, you can only make 

educated guesses about what the structure might be. It’s one 

of the unique strengths of this program that we can provide 

a very thorough characterization of catalysts as we build and 

use them.”

That’s helped guide experimentalists Sadow and 

Slowing work towards common research goals, refining 

the designs of both the mesoporous structures and the 

catalysts themselves. 

“Honestly, without Marek we’d be flying blind,” said 

Sadow. 

“We of course want these systems to work well, to be 

useful, but we also want to understand how they work,” said 

Pruski. “If we can achieve that understanding, we can engage 

in a rational design of catalytic systems rather than rely on 

serendipity.” 

Theorist3

“We try to help them figure out what exactly 

happens in the middle. It’s a way of verifying 

a n d u n d e r s t a n d i n g t h e i r e x p e r i m e n t a l 

results. ” 

 – Theresa Windus

Three theorists have contributed their computational 

modeling expertise in order to better understand the systems 

the experimentalists are designing. 

One of them, Theresa Windus, an Ames Laboratory 

associate in chemistry, has provided Sadow with computer 

models of the reaction mechanisms of the catalysts he and 

Slowing are building. 

“They have their catalyst, and their reactants and 

end products, but they can’t really see the reaction 

itself occurring. We try to help them figure out what 

exactly happens in the middle. It’s a way of verifying and 

understanding their experimental results, infrared and 

NMR spectra,” said Windus. 

Many times, said Windus, it begins with a dialogue. 

“They’ll ask us to verify some experimental result, and after 

doing the computations, we’ll realize that we’re not getting 

what they think we should. Then we go back to them and 

ask ‘is there another explanation for what’s happening?’ It 

becomes a very synergistic information loop.”

8 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 9

Additionally, Ames Laboratory associate Jim Evans 

has provided Igor Slowing kinetic models describing how 

molecules move within the nanopores of the materials, and 

Ames Laboratory associate Mark Gordon has contributed to 

the group with molecular modeling of chemical processes 

on the surfaces of the materials. 

Taken altogether, Sadow considers the contribution of 

the three an asset to the experimental side.

“I think that you can force systems to behave in certain 

ways,and ask questions about them in theory that you really 

cannot ask in an experiment,” said Sadow. “That helps us 

consider different possible pathways to the same result, and 

which one best describes what’s actually happening.”

World-class catalysis research

“A single person cannot realistically have 

all the skills needed to fully interrogate 

matter. You need many people, many skills.” 

 

– Igor Slowing

Ames Laboratory’s combination of catalysis, spectroscopy 

and theoretical experts creates a widely respected research 

reputation in a field that has far-reaching impact in industrial, 

environmental and medical applications.

“When I first began my research group’s work, I only 

felt comfortable proposing research that I individually had 

the skill set to accomplish,” Sadow said. “That’s always the 

individual’s limitation. With others’ contributions, the scope 

of what kind of problem you can tackle becomes much 

greater, and that’s the great appeal of our research group.” 

Windus considers it personally gratifying to have impact 

on disciplines outside her own area of expertise. “Catalysts 

are a lot of fun,” she said. “They are amazing compounds 

that make perfectly impractical reactions viable, useful and 

doable, and I enjoy making contributions to applied science.”

 And in a broader sense, Slowing believes collaboration is 

also fundamental to success in today’s research world.

“It’s a huge value, the way science is right now. You can 

try to master as many different things as you can, but a single 

person cannot realistically have all the skills needed to fully 

interrogate matter. You need as many different specialists in 

as many diverse areas as possible to be successful.”

According to Pruski, Ames Laboratory has continued to 

lead in the field of catalysis because of the synergistic efforts 

of world-class researchers. 

 “We don’t work together just because we all happen to 

be here in one place. The synergy of this program is truly 

vital, and real.”

Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research w Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research w Chemist2 + NMR Spectroscopy + Theorist3 = World-class Catalysis Research
10 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 11

Graduate research assistants Daniel Freppon, left, and Brett Boote in Emily Smith’s research group use Raman 

spectroscopy to study growing corn plants. The technology allows measurement of chemical composition within the 

plant without disrupting its growth cycle.

iomass holds great promise as a petroleum 

replacement, but unlocking its true potential 

remains a puzzle. A group of researchers at Iowa 

State University and Ames Laboratory hope to 

develop the pieces of that puzzle to create a clearer picture 

of what takes place within a plant and how that applies to its 

downstream uses as biomass.

The $1.8 million, three-year project, funded by the 

Biological and Environmental Research program within 

the Department of Energy’s Office of Science, brings 

together a diverse team of Iowa State plant scientists 

and computational experts, as well as analytical chemists 

from Ames Laboratory. The group will explore the 

fundamental ways plants produce and store energy, how 

to potentially optimize those metabolic processes, and 

then compile the vast amounts of information collected 

in an accessible format.

“It’s very fundamental science,” said Basil Nikolau, 

director of ISU’s Center for Metabolic Biology and one of 

the principal investigators on the project. “Everyone can 

easily recognize a plant, but as you use ever more powerful 

microscopes to look at it in more minute detail, down to the 

molecular level within individual cells, you lose context of 

it as a plant. So we’re looking for a way to represent these 

details within the overall context of the plant.”

Plants use photosynthesis, a process fundamental for 

most life forms on Earth, to capture sunlight and convert it 

to chemicals. But how does that happen? 

“We know the initial chemistry involves separating 

charged particles across a membrane,” Nikolau said. “At its 

core, this project will develop analytical imaging technologies 

to visualize the organization and dynamics of the membrane 

that enables this eloquent dance of molecules in and across 

the membrane to convert sunlight to chemistry.”

Though not useful as a biomass source, the team is 

studying Arabidopsis as a model system. The plant’s genome 

has been mapped and it readily lends itself to study. The 

group is also studying corn, another plant with a vast 

amount of genetic background information, and a crop that’s 

important to Iowa and as a potential biofuel source.

“You can grow it in a small space and it grows quickly,” 

Nikolau explained of Arabidopsis, “so you can produce six 

to eight generations in a year. It’s an ideal plant to study, 

and what we discover is generally applicable to other crops 

as well.”

Specifically, the group is using Arabidopsis plants 

that have been genetically altered to boost autophagy, a 

process plants use to survive resource (carbon or nitrogen) 

limitations.They’ll look at how the plants use a vesicle 

called an autophagosome to conserve biomass and energy to 

survive the resource deficiencies.

Analysis of the plant material relies on the technical 

expertise of a cadre of Ames Laboratory researchers. Using 

techniques such as Raman spectroscopy and stimulated 

emission depletion (STED) fluorescence lifetime imaging 

as well as more traditional mass spectroscopic methods, 

they are able to generate detailed information of not only the 

chemical makeup within the plant, but also the processes 

and changes taking place within the living plant throughout 

its growth cycle.

“Ideally, we want to be able to measure the plant as 

it’s actually growing, without disrupting it or extracting 

Solving the Biomass Puzzle

BY KERRY GIBSON

B

Iowa State University plant scientists (l-r) Eve Syrkin Wurtele, 

Basil Nikolau and Diane Bassham display plant materials being 

studied in a campus greenhouse where the plants are grown. 

“we want to visualize ...this eloquent dance of molecules in and across 

the membrane ...” Basil Nikolau,

Director of ISU’s Center for Metabolic Biology
12 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 13

material,” said Emily Smith, Ames Laboratory scientist and 

ISU associate professor of chemistry. “That means using 

imaging techniques that provide exquisite spatial resolution 

that shows you structures and molecules. You also want to 

get chemical information, to know exactly what chemical 

compounds are present. “

“The STED gives us good spatial resolution so we can 

look at subcellular structures,” Smith continued. “The 

Raman imaging gives us the chemical analysis so we know, 

for example, what fatty acids are present.”

In addition to these techniques by Smith’s group and 

ISU researcher Jacob Petrich, the team is aided by ISU 

associate professor of chemistry Art Winter who has 

developed molecular probes that selectively “light up” or 

“turn on” certain elements within the cell that can then be 

captured by the STED imaging. Ames Laboratory scientists 

Sam Houk and Young-Jin Lee provide additional chemical 

analysis through advanced mass-spectroscopy methods, and 

provide a means of validating the images obtained by the 

other imaging technologies.

“One of the downsides to using the techniques we’ve 

developed is that you can get so much information that one 

person couldn’t begin to sort out what’s important,” Smith said. 

“That’s where the computational techniques developed by Eve 

Syrkin Wurtele and Diane Bassham come into play to sort out 

the needle of useful information in the haystack of data to 

address the particular biological question we’re posing.”

Wurtele and Bassham, both professors of Genetics, 

Development and Cell Biology at ISU, use an integrated 

experimental/biocomputational approach to understand the 

factors that regulate plant development and composition. 

That includes an award-winning computer visualization 

program – yep, a video game – called Meta!Blast. Data can be 

imported into the program and it provides a visual depiction 

of what’s taking place within the plant at the appropriate 

cellular or molecular scale. 

“The idea is that you have this visual environment 

that’s new to most people and you can do things like scan 

structures or molecules if you don’t understand them, 

get an explanation of the analytical technologies, and 

see multiple vantage points,” Wurtele said. “The various 

chemical and biological (analytical) techniques let you 

create an image of the plant and its molecular components 

that is at a resolution from a multicellular level, like the 

surface of a leaf, to the cellular, into the organelles within 

individual cells, and ultimately the individual molecules.”

All involved say the project perfectly melds the strengths 

of ISU and Ames Laboratory.

“In our group, we’re all experts in our own domains, 

but I don’t think there’s one person who fully understands 

the other people’s technologies,” Wurtele said. “The idea 

behind this is to create a system where the actual data that’s 

obtained at different resolutions and spatial compartments 

is integrated so that anyone is able to access the data in an 

understandable form.”

“It’s a highly collaborative project,” Nikolau added, “and a 

very good fit between the biological and the analytical sides.”

“We developed these various analytical techniques for 

other purposes,” Smith concluded. “With this project, 

we’re able to apply them to biological materials. ISU is 

extremely strong in plant science and Ames Lab has vast 

analytical expertise, and it’s been great to see this synergy 

develop. Hopefully we can leverage that down the road on 

future projects.”

This image from the Meta!Blast program shows structures 

within the cells of plant. The program is used to visually 

represent huge volumes of data collected from living plants to 

accurately depict what takes place chemically and physically 

within the plant.

All involved say the project 

perfectly melds the strengths 

of ISU and Ames Laboratory.

n just a little over a year of operation, Ames 

Laboratory’s dynamic nuclear polarization (DNP) solidstate nuclear magnetic resonance (NMR) spectrometer 

has successfully characterized materials at the atomic 

scale level with more speed and precision than ever possible 

before. Spectra for materials important to catalysis, solar 

energy, and hydrogen storage have helped scientists better 

understand how these materials work.

Conventional NMR detects the responses of atomic 

nuclei to direct excitation by radio frequency waves. DNPNMR offers faster and more detailed spectra over traditional 

NMR by first exciting unpaired electrons at their microwave 

resonance frequency and then transferring the resulting spin 

polarization to the material’s nuclei. This additional step 

results in much stronger signal intensities from these “hyperpolarized” nuclei than is available by conventional means.

The advanced capabilities of DNP-NMR have already 

made it possible for Ames Laboratory NMR experts to 

answer questions that were out of reach before. 

For example, in a paper in the Journal of the American 

Chemical Society, Ames Laboratory scientist Marek 

Pruski and his research team reported on DNP studies 

of natural abundance 17O in several materials. Oxygen is 

practically undetectable by conventional NMR due to its 

I

DNP-enhanced 17O (a and b) and 195Pt 

solid-state NMR spectra (c) of surface 

species. In (a) a natural abundance 1H-17O 

HETCOR spectrum of silica surface 

allowed for the distinction of hydrogenbonded and non-hydrogen-bonded silanol 

sites. In (b) natural-abundance 17O NMR 

enabled, for the first time, the detection of 

defect sites in MOFs. In (c) 195Pt NMR 

experiments of surface-bound Pt sites 

enabled the unambiguous characterization 

of their binding environment. 

Higher Speed, 

More Precision

 BY BREEHAN GERLEMAN LUCCHESI
14 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 15

low natural abundance and quadrupolar nature. “The signal 

enhancement that DNP provides, allows for detection of 

17O without enrichment,” said Pruski. “The detection of 17O 

nuclei was among our key targets early on, because oxygen is 

one of the most ubiquitous elements in materials.”

Frédéric Perras, Pruski’s colleague and Ames Laboratory’s 

Spedding Postdoctoral Fellow, used DNP to hyper-polarize 

1

H nuclei, and subsequently transferred 1H polarization to 17O, cleverly using a scheme called PRESTO, which was 

published over 10 years ago and then nearly forgotten in the 

NMR community. Perras has since used DNP-enhanced 

17O solid-state NMR to characterize mesoporous silica 

nanoparticles (MSNs) and metal organic frameworks 

(MOFs) without expensive isotope enrichment (shown in 

the figures on page 13). 

Pruski and his team, which also includes Ames Laboratory 

scientist Takeshi Kobayashi, use DNP-enhanced spectra of 

other nuclei, such as 15N, 29Si, 27Al, 195Pt, and 207Pb, to make 

key characterizations of a variety of other materials prepared 

at Ames Laboratory. 

They collaborate with Aaron Sadow’s and Igor Slowing’s 

research groups on the design and testing of new types of 

supported catalysts, as well as new polarizing agents that 

may offer even more improvement in DNP measurements. 

They also work together with Vitalij Pecharsky and coworkers on understanding the solid-state transformations 

in complex metal hydrides. The ‘DNP contingent’ has been 

further strengthened by Aaron Rossini, who recently joined 

the Ames Laboratory as a faculty scientist. Rossini’s interests 

include DNP characterizations of novel materials as well as 

DNP method development. 

“Hardly a week passes where we don’t get a contact 

from other researchers about DNP, and the instrument is 

operated practically non-stop,” said Pruski. “Our external 

collaborations include Iowa State University, Argonne 

National Laboratory, Northwestern University, Washington 

University, University of Delaware, University of Lille (Lille, 

France), University of Wisconsin and Purdue University, 

and the list continues to grow.” 

One important next step is enhancing the capabilities of 

DNP by designing new pulse sequences, instrumentation, 

highly efficient polarizing agents and improved sample 

formulations, in order to open new doors to even faster, 

detailed measurements of materials’ properties. Pruski’s 

team is engaged in this effort. 

“DNP was invented by physicists and then first widely 

used by researchers to characterize biological systems, but 

I think many would agree that the primary beneficiaries of 

DNP are materials scientists and chemists,” he said. “The 

technique is particularly well suited for studying the surfaces 

of materials. But, it’s still early and much work is needed to 

improve the technique.”

Ames Laboratory scientist Marek Pruski, left, 

and Ames Laboratory postdoc and Spedding Fellow 

Frédéric Perras stand next to the DNP NMR equipment.

Hardly a week passes 

where we don’t get 

a contact from other 

researchers about DNP, and 

the instrument is operated 

non-stop ...

Takeshi Kobayashi, left, looks on while Frédéric Perras 

loads a sample into the DNP NMR equipment.
ccording to the U.S. Environmental Protection 

Agency, the United States produced 254 million 

tons of municipal solid waste in 2013. And 

though 87 million tons of that material from 

landfills was diverted through recycling and composting, 

what if the nation could do better? What if landfills could 

become local sources of clean energy production? Better 

yet, what if all waste streams, like those from agricultural, 

livestock, and food production, could essentially become 

fuel refineries at a local level?

It’s a question being asked by a collaboration of national 

laboratory researchers who want to create energy conversion 

technologies designed to mine the carbon out of waste 

processes that traditionally have been an environmental 

burden to the planet and a disposal headache for humans.

“The idea of using waste as energy source really isn’t new,” 

said Cynthia Jenks, assistant director of Scientific Planning 

and division director for Chemical and Biological Sciences 

for Ames Laboratory. “For example, some municipal and 

regional utilities already burn landfill waste as a source 

for electrical power. But we think there are better, cleaner 

and more efficient ways to get at that carbon and use the 

potential energy from it.”

A new concept was born of the Big Ideas Summit, held 

by the Department of Energy and its national laboratories 

in 2015. The effort, being co-led by Ames Laboratory and 

Pacific Northwest National Laboratory, is a collaboration of 

12 national laboratories to find new catalytic technologies 

that can efficiently produce biofuel from waste streams. 

The goals are specific. Make the technology as simple 

as possible, yet adaptable to diverse waste streams. Locate 

it right at the waste stream source, whether it’s a landfill, 

livestock farm or commercial facility. Make it easy and 

economical to produce and deliver through the use of 

modular manufacturing. 

 “The idea brings together a lot of overlapping interests: 

chemical research, applied engineering, modular 

manufacturing, waste management, agriculture, industry, 

A

What if America’s next big fuel source is its trash?

BY LAURA MILLSAPS

Waste Stream to Energy Source: 

“That’s really the ‘big idea,’” said Jenks. 

“Where there is waste, there is energy.” 

16 Inquiry Issue 2 | 2015 Inquiry Issue 2 | 2015 17

and energy-sector investors. It’s a complex idea with a lot of 

moving parts, but one that we think will get us a lot closer to 

accessing the potential energy in these underused resources, 

and a lot closer to the nation’s sustainable energy production 

goals,” said Jenks.

To meet the goal, the participating national laboratories 

will pool their skills in materials and chemical sciences, 

high-performance computing, engineering, and applied 

technology. Ames Laboratory will lend its expertise in 

catalysis to the project through its Chemical and Biological 

Sciences Division. Scientists Igor Slowing and Aaron Sadow 

have already done extensive work in creating catalysts that 

are able to convert carbons, by placing catalytic agents on 

high-surface-area nanomaterials. They want to develop 

processes that make possible the controlled decomposition 

of waste polymers into useful hydrocarbons.

“A large amount of the waste that goes into landfills 

is polymers...plastics. These are very carbon rich, very 

processed materials, and if we were to be able to convert 

that waste into new, useful compounds or energy, that 

would make much better use of them,” said Sadow. “Right 

now, we’re wasting all that carbon. It’s just sitting there in 

the trash.” 

Sadow and Slowing will also be applying similar techniques 

to the conversion of wet sludge and agricultural wastes. 

Sadow said the scientific challenges are complex, with 

a need for chemical reactions that can be highly efficient, 

operating at low temperature and low pressure. They will 

also need to be capable of adapting to changes in the raw 

material feeding them. 

“Any waste stream is very mixed, and its composition varies 

over time,” said Sadow. “We can physically sort and then 

convert, but then there’s that separation step. We don’t really 

know how to chemically convert mixtures in general. That is 

a really big, interesting, fundamental challenge that research 

hasn’t yet tackled, and that’s exciting to contemplate.”

While the group estimates that these localized biofuel 

refineries would produce small quantities of biofuel—an 

average of the equivalent of 125 barrels of oil per day—the 

collective impact could be staggering. Transforming the 

available national waste streams into fuels and other useful 

chemical products could translate to the equivalent of 2.7 

billion barrels of oil per year, or 40 percent of the nation’s 

annual crude oil use. 

“That’s really the ‘big idea,’ ” said Jenks. “Where there 

is waste, there is energy. We believe that the collective 

expertise of the national labs, including the chemical 

research strengths of Ames Laboratory, puts that big idea 

within reach.” 

“A large amount of the waste that goes 

into landfills is polymers...plastics. 

These are very carbon rich, very 

processed materials, and if we were to 

be able to convert that waste into new, 

useful compounds or energy, that would 

make much better use of them. Right 

now, we’re wasting all that carbon. It’s 

just sitting there in the trash.”

Aaron Sadow
ight out of the past 10 years, Ames Laboratory 

chemist Aaron Sadow has mentored a Science 

Undergraduate Laboratory Internships (SULI) 

student. Sometimes the mentorship has been for the 

10-week summer program and sometimes for the 16-week 

semester program. On occasion, he’s mentored more than 

one student at a time. 

When asked why he keeps coming back to the SULI 

program, Sadow, who is also associate professor of chemistry 

at Iowa State University (ISU), responded, “SULI is an 

excellent program for everyone involved. Mentors benefit 

from having the opportunity to help train future scientists to 

do great science, graduate students benefit from having the 

opportunity to work with excited undergraduate students, and 

interns benefit from research opportunities that may result 

in published research papers that could lead to additional 

research funding for the mentor’s program.”

Including Sadow’s students, Ames Laboratory scientists 

featured in this issue of Inquiry have hosted more than 50 

students and faculty from 34 universities, colleges and 

community colleges around the country. 

Holding a close second to Sadow’s impressive record 

of commitment to Ames Laboratory’s science internship 

programs is Ames Laboratory scientist and associate professor 

of chemistry at ISU Javier Vela. But in addition to hosting 

several SULI students, for the past six years Vela has hosted 

two Visiting Faculty Program (VFP) teams, which consist of 

a faculty member and up to two students. With a focus on 

growing a diverse workforce for the Department of Energy’s 

national laboratories, VFP teams come from institutions 

historically underrepresented in the research community.

“It is only because of this program that we’ve have had an 

opportunity to collaborate with the principal investigators at 

these institutions,” said Vela, who was a 2014 recipient of the 

Stanley C. Israel Regional Award for Advancing Diversity in 

Chemical Sciences. “And most of the students we’ve hosted 

would never have thought about coming here. They’ve been E

BY STEVE KARSJEN

Chemists Leave 

Their Mark on 

Future Scientists 

18 Inquiry Issue 2 | 2015 Inquiry Issue 

2 | 2015 19

able to learn more about our Laboratory, university, city, and 

state. It’s been a good experience all-around.”

Javier Grajeda, a SULI intern in 2011, epitomizes the 

importance of internship programs like VFP that are focused 

on diversity. Vela met Grajeda, a student at the University 

of Texas at El Paso (UTEP) at a Society for Advancement 

of Chicanos/Hispanics and Native Americans in Science 

(SACNAS) conference. A discussion of Vela’s work in 

inorganic chemistry piqued Grajeda’s interest so he applied 

for the summer 2011 SULI program. During his short 

internship, Grajeda co-authored a paper with one of Vela’s 

graduate students, which was published in the journal 

Chemistry of Materials. In addition to working in his lab, 

Vela said Grajeda also continued working with scientists at 

UTEP and then traveled to China to do research. When 

it was time to apply for graduate school for his Ph.D. in 

chemistry, Grajeda was accepted at the University of North 

Carolina at Chapel Hill. At the same time, he was awarded 

a highly competitive three-year fellowship through the 

National Science Foundation Graduate Research Fellowship 

Program. When asked about the key to his success, Grajeda 

said, “Working under Dr. Vela has had a great impact on my 

career, and I’m grateful for having been given the opportunity 

to participate in the SULI program.”

Although he would have preferred to have had Grajeda 

enter graduate school at Iowa State, Vela takes a long view 

of the situation and said ultimately “everyone wins with the 

DOE’s internship programs” because they help facilitate the 

growth of students like Grajeda, who may end up working as 

scientists at DOE laboratories. 

Ames Laboratory scientist Igor Slowing, who has 

mentored 10 SULI students since 2012, echoes Vela’s 

comments. Slowing said internships offered through SULI, 

VFP and the Community College Internship (CCI) program 

are a “good advertisement” for Ames Laboratory. “What we 

are doing in the DOE’s labs is communicated to more people, 

which in turn helps universities and communities learn more 

about the DOE and its national labs, which then helps the 

American taxpayer understand what we’re doing with their 

taxpayer dollars,” said Slowing. 

 

... everyone wins with the DOE’s 

internship programs ... 

Javier Vela, Ames Laboratory scientist 
Ames Laboratory

111 Technical and Administrative Services Facility

Ames, Iowa 50011-3020

515-294-9557

www.ameslab.gov

2015

Issue 1

Science & Technology at the Ames Laboratory

Issue 2