The Future of Stardust Science

A. J. Westphal1, J. C. Bridges2, D. E. Brownlee3, A. L. Butterworth1, B. T. De Gregorio4, G.

Dominguez5, G. J. Flynn6, Z. Gainsforth1, H. A. Ishii7, D. Joswiak3, L. R. Nittler8, R. C. Ogliore9,
R. Palma10,13, R. O. Pepin10, T. Stephan11, M. E. Zolensky12

1
Space Sciences Laboratory, U. C. Berkeley, Berkeley CA, westphal@ssl.berkeley.edu
2
Space Research Centre, Dept. of Physics & Astronomy, University of Leicester, UK
3
Department of Astronomy, University of Washington, Seattle WA
4
U. S. Naval Research Laboratory, Washington DC
5
California State University at San Marcos, San Marcos, CA
6
State University of New York, Plattsburgh, NY
7
Hawaii Institute of Geophysics and Planetology, University of Hawaii at Manoa, Honolulu, HI
8
Department of Terrestrial Magnetism, Carnegie Institute of Washington
9
Washington University in St. Louis, St. Louis MO
10
Department of Physics, University of Minnesota, Minneapolis, MN
11
Department of the Geophysical Sciences, The University of Chicago, Chicago, IL
12
ARES, NASA JSC, Houston, TX
13
Department of Physics and Astronomy, Minnesota State University, Mankato, MN

Abstract
Recent observations indicate that >99% of the small bodies in the Solar System reside in its
outer reaches – in the Kuiper Belt and Oort Cloud. Kuiper Belt bodies are probably the best
preserved representatives of the icy planetesimals that dominated the bulk of the solid mass
in the early Solar System. They likely contain preserved materials inherited from the
protosolar cloud, held in cryogenic storage since the formation of the Solar System. Despite
their importance, they are relatively underrepresented in our extraterrestrial sample collections
by many orders of magnitude (~1013 by mass) as compared with the asteroids, represented by
meteorites, which are composed of materials that have generally been strongly altered by
thermal and aqueous processes. We have only begun to scratch the surface in understanding
Kuiper Belt objects, but it is already clear that the very limited samples of them that we have in
our laboratories hold the promise of dramatically expanding our understanding of the
formation of the Solar System. Stardust returned the first samples from a known small solar-
system body, the Jupiter-family comet 81P/Wild 2, and, in a separate collector, the first solid
samples from the local interstellar medium. The first decade of Stardust research resulted in
more than 142 peer-reviewed publications, including 15 papers in Science. Analyses of these
amazing samples continue to yield unexpected discoveries and to raise new questions about
the history of the early Solar System. We identify 9 high-priority scientific objectives for future
Stardust analyses that address important unsolved problems in planetary science.
INTRODUCTION

2016 marks the 10th anniversary of the return to Earth of the Sample Return Capsule from
Stardust, the first mission to capture and return solid extraterrestrial samples from beyond the
Moon. Stardust returned the first cometary solids ever sampled directly from a comet’s coma,
and a separate collector that was exposed to the stream of interstellar dust and which
probably (but not yet certainly) contains a handful of tiny local interstellar rocks, the first ever
identified. This low-cost, high-risk mission – really two missions, in one spacecraft – has been
extraordinarily successful by any measure. The first decade of Stardust research resulted in
more than 142 peer-reviewed publications, including 15 papers in Science. Unexpected
discoveries have led to major revisions of our understanding of structure and history of the
early Solar System and analyses of these amazing samples continue to yield unexpected
discoveries and to raise new questions about the history of the early Solar System. For
example, the discovery of highly refractory minerals, minerals implanted with high
concentrations of implanted noble gases, and “microchondrules” implies large-scale outward
transport of material in the disk, from the inner solar system all the way out to the Kuiper Belt.
Like archaeologists investigating human origins through the study of rare ~4 Ma old fossils of
ancient hominids in Ethiopia, cosmochemists are investigating our own cosmic origins through
the study of rare ~4.6 Ga old “fossil” solar-system building materials, going a thousand times
further back in time than our archaeologist colleagues. One Stardust investigation, still
ongoing, inspired a multitude of “citizen science’’ projects that productively collaborate with
thousands of amateurs in achieving important science goals across a variety of disciplines.

Because they are a rare, finite resource, Stardust samples pose logistical and technical
challenges beyond those involved in analyzing most other extraterrestrial materials, such as
meteorites, which are far larger and far more abundant. The analysis of a single complex 10
µm diameter particle, typically <1 ng (10-9 g) in mass, can easily consume a year or more of
effort by a small research group. Long-term investment by NASA and other agencies in
improvements in analytical instruments and techniques, and in sample handling and
preparation, which started with Apollo, has yielded spectacular advances in our understanding
of the early Solar System, but it is equally clear that the research on Stardust samples, to
date, has only scratched the surface and many fundamental questions remain about the
nature of these samples. With Stardust cometary samples, we are now perhaps where we
were in approximately 1960 in the study of meteorites. For example, we do not know the bulk
composition of comets with sufficient accuracy to be able to make a sensible comparison with
other extraterrestrial materials. A full understanding of the nature of these astonishing
samples will require patience and perspective.

With dust particles from the Stardust interstellar collector, the situation is even more striking.
Here we are perhaps where we were in approximately 1800 with meteorites, just after they
were proposed to be cosmic in origin by Ernst Chladni, because it is not yet proven that any of
the Stardust interstellar dust candidates identified so far are in fact interstellar in origin.
Fundamentally, the reason is simple: as small and challenging as the cometary samples are,
interstellar dust samples are several orders of magnitude more challenging. Typical
interstellar dust particles are at least a thousand times less massive than typical cometary
particles, and the total number of particles is <<1% of number of particles in the cometary
collection.

A decade on, this is perhaps a good time to ask three questions: What have we learned from
the Stardust mission? What role will the analyses of Stardust samples play in the future of
Planetary Science and Astrophysics? What resources will be needed to carry out these
analyses? We will organize the responses to the last two questions around a list of unsolved
problems in planetary science and astrophysics that can be addressed by analyzing Stardust
mission samples. The goal of this paper is to provide an overview of work that has and is
being done on the comet and interstellar dust samples and provide some insight into
investigations that can be done in the future. The focus is on Stardust mission samples but
many of findings and discussions are clearly important to the analysis of nonvolatile
components that will be obtained on future sample return missions.

This paper is the product of a workshop that was held near the UC Berkeley campus on July
26-27, 2015, just prior to the 78th annual meeting of the Meteoritical Society. The workshop
was supported by NASA and sponsored by the Curation and Planning Team for
Extraterrestrial Materials (CAPTEM), a NASA advisory committee.

STARDUST SAMPLES IN CONTEXT

A central goal of the field of cosmochemistry is to understand the formation and evolution of
the Solar System based on clues preserved in ancient and primitive extraterrestrial materials.
The period of formation of the major and minor planetary bodies during the first few million
years of Solar System history is particularly challenging because this period can only be
studied using clues derived from the analysis of relatively rare samples of material that formed
at that time, and that have avoided subsequent alteration or annihilation due to exposure to
heat or water. The clues are uncovered through use of sophisticated laboratory instruments
that must be well-suited to the demanding nature of the samples. Beginning in the 1950’s,
and dramatically accelerated by investments during the Apollo era, the modern field of
cosmochemistry cut its teeth on the study of meteorites, which are by many orders of
magnitude the most readily available extraterrestrial samples. Thanks to ongoing commitment
to meteorite collection campaigns such as ANSMET (Antarctic Search for Meteorites, active
since 1976), many tons of meteorites exist in the worldwide collections (although to be sure
some rare or unique meteorites exist in only ~gram quantities). Mineralogic and petrographic
studies, measurements of elemental and isotopic composition, analyses of organics and noble
gases, and others, have now reached an extraordinary level of sophistication. One
consequence of these improvements was a dramatic reduction in the required size of samples
for a given type of measurement, sometimes by orders of magnitude. Improvements in
sensitivity and resolution led to discoveries that otherwise would have been impossible, such
as the discovery of trace quantities of ancient “presolar” grains in primitive meteorites (e.g.,
Zinner 2014).
Fig. 1. Masses of extraterrestrial sample collections versus heliocentric distance of formation.
Existing collections are shown in bold, collections from missions in progress (Hayabusa 2,
OSIRIS-REx) or proposed (New Frontiers Comet Surface Sample Return) are shown in grey.
The mass of the Stardust cometary sample is tiny compared to the meteorite collection but is
the first known to have originated outside the inner Solar System. Extraterrestrial sample
collections suffer from a severe sampling bias: since Kuiper-belt objects outnumber asteroids
by a factor of ~100, they are relatively undersampled as compared with the asteroids by
>1013. For a sense of potential scale, the recent millimeter-wave ALMA image of the
protoplanetary disk HL Tau is shown, overlaid with the orbits of the Earth and the four solar-
system gas giants. It is not yet known whether the Solar System’s protoplanetary disk was as
extensive as this one. HL Tau image credit: ALMA (ESO/NAOJ/NRAO).

Meteorites are samples of small bodies that are thought to have formed in a relatively narrow
range of heliocentric distances, mostly between 2 and 3 AU, between the present-day orbits of
Mars and Jupiter. The remarkable mineralogical, chemical, and isotopic complexity of the
meteorite collection is itself an important observation, and implies strongly varying conditions
in space (and probably time) in the inner Solar System, with admixing of equally complex
material formed elsewhere. However, astronomical observations of protoplanetary disks, and
especially spectacular new millimeter-wavelength observations by ALMA (Figure 1, Atacama
Large Millimeter/submillimeter Array, almaobservatory.org), show protoplanetary disks
extending to 100 AU or more. The extent of the protoplanetary disk from which our Solar
System evolved is unknown, but it is likely that meteorites sample only a tiny,
unrepresentative fraction of the original protoplanetary disk. Asteroids themselves are now
thought to constitute only a small fraction of the population of small bodies in the Solar
System; recent observations indicate that Kuiper Belt objects, which formed or at least orbit
beyond Neptune, outnumber asteroids by at least two orders of magnitude (Schlichting et al.
2012, Bottke et al. 2005, Farinella and Davis 1996). Analysis of samples formed in outer
regions of the disk is thus required for even a partial understanding of the structure and history
of the Solar System.
We now know of several thousand extrasolar planets. It is clear from the data that there is a
wide variation in the types of planets and distribution of these within extra-solar planetary
systems. How this variation came to be is a very important area of astrophysics and is a
question that analyses of the oldest and arguably most pristine samples of Solar System
building blocks can help to answer.

Starting in 1981, immediately after the pioneering work of Don Brownlee (Brownlee et al.,
1977), the then-future PI of the Stardust mission, NASA has been collecting Interplanetary
Dust Particles (IDPs) in the stratosphere (Warren and Zolensky, 1994). Several lines of
evidence point to a cometary origin for a class of fine-grained IDPs containing anhydrous
minerals, called Chondritic-Porous IDPs (Bradley & Brownlee 1986, Bradley 1994, Bradley et
al. 1999). Because of limitations of the collection technique, no particular IDP can be
unambiguously identified with a specific small body, so the question of their origin(s) is not yet
completely resolved. Larger particles called micrometeorites (e.g., Dobrica et al. 2009,
Noguchi et al. 2015) have been recovered from polar ice and snow (Maurette 1991, 1994,
Duprat et al. 2010). These larger particles are generally more strongly heated during
atmospheric entry and may be altered in the terrestrial environment, especially by leaching.
As a consequence, their origins are less certain, although they probably derive from both
asteroids and comets. Some have been found to have identical fine-grained components to
Chondritic-Porous IDPs and, thus, sample sources that are most likely cometary (Noguchi et
al. 2015).

The Stardust mission collected materials from the coma of the Jupiter-Family comet Wild 2 in
2004 (Brownlee et al. 2003a). The total mass of the collection, >300 µg (Hörz et al. 2006), is
orders of magnitude smaller than even the smallest meteorite. But despite its diminutive size,
the “lever arm” of this sample collection is enormous. Although the Stardust spacecraft
collected material from Wild 2 while it was in the inner Solar System, Wild 2 almost certainly
formed in the Kuiper Belt (it has been in its present orbit only since 1975, when it had a close
encounter with Jupiter). So the Stardust cometary samples are the first from a known solar-
system body that likely formed in the outer Solar System (Fig. 1). Recent studies of gas
emitted from Wild 2 show that it has a frozen volatile content that is typical of comets from the
Kuiper Belt (Dello Russo et al. 2014). Because we have been studying meteorites for
decades and have literally tons of material in our collections, we have a bias towards thinking
of these as typical of small solar-system objects, though in fact, they are not. More than 99%
of small bodies in the Solar System probably resemble objects like Wild 2: recent observations
imply that Kuiper Belt Objects outnumber asteroids by more than two orders of magnitude
both in number and by mass (Schlichting et al. 2012, Bottke et al. 2005).

planets and undifferentiated comets interstellar dust

differentiated asteroids
asteroids

Parent body

melting and major minor to none none

differentiation

parent-body major major to minor none

thermal
metamorphism

aqueous alteration major major to minor moderate to none

shock major to minor major to minor minor to none

Nebula

hot evaporation major minor?

and condensation

chondrule-forming major major?

process or other
nebular heating

radiation minor? major?

processing (e.g., GEMS)

cold condensation minor? major?

and evaporation (e.g., organics)

ISM

hot evaporation minor? (e.g., major?

and condensation enstatite whiskers)

radiation major? (e.g., major?

processing GEMS?)

cold evaporation minor? major? (e.g., major?

and condensation GEMS?)

Circumstellar

hot evaporation minor minor? (e.g., minor?

and condensation presolar grains)

radiation minor? minor? minor?

processing

cold evaporation minor? minor? minor?

and condensation
Table 1. Processes that control chemistry and mineralogy of extraterrestrial solids, , and
which may be recorded and preserved in them.

Interest in the degree to which our extraterrestrial sample collections are representative of all
Solar System bodies is driven by the different environments they likely sampled and the
different processing they underwent. In Table 1, we highlight the different processes affecting
classes of planetary bodies and interstellar materials. The processes that control the
mineralogy of cometary and interstellar dust overlap those that control the mineralogy of
meteorites, but generally those that are minor in asteroids are major in comets, and vice
versa.

Advances in laboratory instrumentation

FTIR

SIM
10 µm

SX
wet chemistry SFTIR

RF
/SX
optical microscopy

RD
1 µm

SEM/ED
X EM
PA

100 nm
NanoSIMS
NanoFTIR
spatial resolution

Auger
10 nm SE STXM
M
im
agi RIMS
ng
elements mineralogy pSTXM

1 nm isotopes imaging
APT
TE
M HIM
AC-TEM
1 Å

1969-72 1980’s 2004 2010 2023 2030’s

Meteorites
IDPs
cosmic Stardust
spherules Genesis Hayabusa
Apollo OSIRIS-REx
1876

(Comet Surface
Sample Return)

Fig. 2 Illustration of the advances in spatial resolution of various microanalytical techniques,

superimposed on a timeline of returned extraterrestrial samples. See Appendix for glossary
of terms.
Unlike most NASA missions, the instrument suite of the Stardust mission was relatively
simple. The mission carried particle impact detectors and a time-of-flight impact mass
spectrometer but its primary goal was to use passive collectors to capture and return solid
materials from the coma of a specific comet, 81P/Wild 2, and, in a separate collector,
interstellar dust from the local interstellar dust stream. Laboratory identification of phases in
Wild 2 samples is generally more straightforward and diagnostic than identification through
remote observations in cometary comas. In this sense, Stardust provides “ground truth” for
astronomical observations. Most of the analytical sophistication of the mission was – and
continues to be – on the ground after recovery. Researchers analyze samples using
instruments that could never be flown in space, such as synchrotrons – X-ray and infrared
microprobes the size of shopping malls. Instruments on Earth are unconstrained by the mass,
power, and reliability requirements imposed by spaceflight and need not exist at launch. With
careful curation (Zolensky et al. 2008a, Frank et al. 2013), samples can be analyzed decades
after return, taking advantage of instruments with capabilities that might not be imagined
during mission planning. Perhaps most importantly, measurements can be repeated by
different instruments in different laboratories to confirm (or disprove) results – the backbone of
the scientific process. Results from analyses often lead to refined approaches to investigate
issues that were not previously known. The discovery of presolar grains in meteorites is an
excellent example of what can ultimately evolve from complex, often confusing, and ever
improving data.

Challenges in Stardust sample analysis

Stardust samples pose challenges that are unfamiliar to those accustomed to studying other
sample collections. Unlike the meteorite, IDP, or polar micrometeorite collections, which are
more readily available because new samples are continually raining from the sky, the samples
returned by Stardust are a small and finite resource. As a consequence, the process for
requesting, preparing, and allocating samples to researchers is deliberately painstaking and
can be frustratingly slow. The highly demanding nature of the samples requires cutting-edge
instruments that are often highly oversubscribed, as well as the development of novel sample
handling techniques and procedures to prepare the samples for analysis in those instruments.
While the Stardust cometary collection suffers from this challenge to a certain extent, the
interstellar dust collection demonstrates it in the extreme. The total number of “large”
particles, of order 1 picogram (10-12g) in mass, is probably no more than a dozen, and the total
mass of the interstellar collection is estimated to be less than one-millionth that of the Stardust
cometary collection.

Although great sample-derived insight on the origin of comets has come from the first decade
of study, it is clear that the research on Stardust samples has only scratched the surface. We
do not yet understand the diversity of materials that compose even this one comet, Wild 2. It
appears that Wild 2 contains abundant “xenoliths” (foreign rocks) from all over the Solar
System, including minerals that form at high temperatures (Zolensky et al. 2006); however,
observations of the stratified structure of comet Churyumov-Gerasimenko by the ESA Rosetta
mission implies that its formation was an episodic, gentle, and cold process (Massironi et al.
2015).. Is transport in a turbulent disk consistent with both observations, and could these
“xenoliths” really have been transported in such large quantities from the inner Solar System?
Or is it possible that they were somehow formed in the outer Solar System?

Answers to these questions will yield important advances in our understanding of the early
Solar System, similar to those resulting from the Apollo-era-initiated, long-term NASA
investment in analytical instruments and in sample preparation. More than 95% of the
samples returned in 2006 are still available for analysis.

The Stardust mission also served as a catalyst for the development (or refinement) of
analytical techniques to maximize the scientific payout of the mission. Because there are other
sample return missions, either in flight or in the proposal stages (OSIRIS-REX, Hayabusa 2,
Comet Surface Sample Return), the techniques and expertise developed through NASA
support of laboratory analysis of returned samples will continue to be essential to the success
of these missions. Investment into instrumentation capable of processing cometary samples
yields a double dividend as the same instrumentation advances are applied to meteorites and
IDPs.

SCIENTIFIC OBJECTIVES FOR THE NEXT DECADE OF STARDUST RESEARCH

Here we summarize our view of the highest priority scientific objectives in the coming decade
for analyses of Stardust samples. Although a great deal was learned from the remote
observations of comet Wild 2 during the flyby by the Stardust spacecraft, we focus here on the
primary goal of the mission: discoveries arising from the first laboratory analyses of bona fide
cometary solid materials collected from a known comet whose activity and orbit is typical of
Jupiter family comets. Because the interstellar collection is several orders of magnitude more
challenging than the cometary collection, even after a decade we are still in the infancy of its
analysis, and there are many uncertainties;the evidence for interstellar particles in the aerogel
collector is still circumstantial and remains to be confirmed through further analyses.
Objective 1: Determine modal mineralogy of Wild 2 for comparison with primitive
chondrites and CP-IDPs

Question and Objective measurement instrument sample sample

requirements frequency

1 What are comets made of? Major modal mineralogy (coarse analytical TEM, keystone, common
Determine modal mineralogy grains, fines, Type II chondrules and µXRF/XRD, ultramicrotome
for comparison with primitive chondrule fragments, sulfides, metal, XANES, EBSD sections
chondrites and CP-IDPs Kool grains, organics, carbonaceous
material), bulk chemistry

Concentration of minor phases analytical TEM, ultramicrotome common

(CAIs, Type I chondrules, Al-rich µXRF/XRD, sections
chondrules, enstatite whiskers, XANES
cubanite, pentlandite)

Concentration of phases exclusive to analytical TEM shielded rare (Kool

CP-IDPs (enstatite whiskers, GEMS, material grains)
Kool grains) (possibly behind unknown
terminal (GEMS,
particles) whiskers)

Concentration of primary analytical TEM, ultramicrotome common

condensation products (LICE/LIME µXRF/XRD sections
olivine, enstatite whiskers)

Summary of objectives
● Determine the relationship of Wild 2 CAIs and meteoritic CAIs
● Determine the relationship between Wild 2 microchondrules and chondrule
fragments and meteoritic chondrules
● Clarify the relationship between Wild 2 and CP-IDPs
● Accurately determine the modal abundance of CAIs
● Accurately determine the relative mix of coarse-grained and fine-grained
components
● Substantially improve statistics of analyses of Kool grains
● Accurately determine the presolar grain abundance
● Accurately determine the enstatite whisker abundance
● Accurately determine the LIME forsterite abundance
● Accurately determine the GEMS and Polyphase Unit abundance
● Determine the abundance of aqueous alternation products (Objective 5)
Technology advances
● High energy-resolution X-ray spectroscopy (e.g., microcalorimetry)
● High spatial-resolution synchrotron mapping with Mg, Al Kα detection
● Improve dust particle accelerator technology to reduce acceleration shock

When taking a first look at the Wild 2 samples a decade ago, it was natural to ask: Have we
seen this material before? Can we recognize materials that we find in other primitive solar-
system materials – in primitive meteorites or in primitive CP-IDPs?

The process of answering this straightforward question is complicated by several confounding

issues. All three collections – primitive meteorites, CP-IDPs and Wild 2 cometary samples –
have been altered since their formation ~4.6 Gy ago by distinct mechanisms and to varying
degrees. Even the most primitive meteorites show signs of aqueous alteration or thermal
metamorphism that took place on the small bodies from which they originated; the finest-
grained components (the “matrix”) in meteorites is the most susceptible to these effects. CP-
IDPs were often heated to incandescence during atmospheric entry, so are thermally altered
and oxidized to varying degrees by reaction with atmospheric oxygen, particularly on their
rims. Wild 2 samples are altered in complicated ways by the effects of capture at 6.1 km/sec
in aerogel or aluminum foil. Nevertheless, an inventory of the materials in returned Wild 2
samples that allows for a first-order comparison to the other collections sets the context for
understanding them.

Major modal mineralogy

The early work on the Wild 2 samples involved a learning curve to develop means of
distinguishing between well-preserved materials and those that had been altered during high
speed capture (Brownlee et al. 2006). Although laboratory capture experiments had been
done previously, this was the first experience with cometary solids, a complex fragile mix of
fine and coarse components. Generally, it was found that components near the ends of
aerogel capture tracks and those larger than a few micrometers were well preserved, often
with a protective cap of compressed SiO2 aerogel. However, all tracks also contained
components that were modified to various degrees from slight to severe in which some
components melted and dissolved in the molten silica that lines the walls of capture tracks
(Ishii et al. 2008a).
Fig. 3: TEM view of a Stardust terminal particle ultramicrotomed section. A) STEM HAADF
image. A large region of mixed aerogel and Stardust is outlined at the top, and additional
“fusion crust” regions are marked with arrows. 1 micron scale bar. B) EDS view of the same
region with Fe (red), Mg (green), Si (blue) showing sulfide in the upper corner and bottom, and
silicate everywhere else.

One of the very first findings of the mission was that the comet was composed of a wide range
of particles that ranged from solid grains, which produced long thin tracks (Type A) made by
non-fragmenting material, to loose fines or unstable materials, which produced broad
(bulbous) tracks (Trigo-Rodriguez et al., 2008, Burchell et al., 2008a). Some of the solid
grains were larger than 50 µm with beautifully preserved interiors (e.g., Nakamura et al.
2008).. One interpretation of the capture process is that the thermal capture effects only
influenced the outer micrometer or less and that larger grains were much better preserved
than smaller ones (Brownlee, Joswiak and Matrajt 2012). The situation is somewhat
analogous to meteorites, where entry heating melts a thin fusion crust but thermal inertia
protects their interiors.
Among early observations was the remarkable finding that isotopically anomalous (“pre-solar”)
grains are rare and that the comet contains fragments of common high temperature nebular
materials, typically found in meteorites. The discovery of micro-chondrules and micro-CAIs
(Ca-Al-rich inclusions) in the comet was quite unexpected and totally at odds with the common
belief that comets formed in isolation from the inner Solar System (McKeegan et al. 2006,
Simon et al. 2008, Chi et al. 2009). In initial studies, the terms “chondrule-like” and “CAI-like”
were used because it was not clear that the usually <50 µm fragments were indeed fragments
of the same components found in meteorites. After nearly a decade of effort, the similarities
are better established: so far all chondrule-like fragments more closely resemble type II
chondrules than Type I chondrules (e.g., Gainsforth et al. 2015), but it remains to be
determined if the Wild 2 chondrules and refractory inclusions do actually sample the same
populations of these nebular components found in chondrites.

Fig. 4: a) HRTEM images of cosmic symplectite (composed of “wormy” grains of

magnetite and pentlandite) in Acfer 094 (ungrouped carbonaceous
chondrite), from Seto et al., GCA, 2008. b) Backscattered electron
image of micro-chondrules in the unequilibrated ordinary chondrite MET
00526 (image credit: Elena Dobrica, UNM). c) Compositional map (from
EPMA data) of Wark-Lovering rim with an included micro-CAI, from Simon
et al., Science, 2011.

Through a tour de force of mission design, the closing speed of the Stardust spacecraft with
comet Wild 2 was only 6.1 km/sec. This relatively low speed was extremely important for
sample science. Because it is within the speed range of two-stage light-gas guns,
experiments can be readily carried out to assess the effect of capture in aerogel (Burchell et
al. 2009, Burchell et al. 2008a, Burchell et al. 2012, Kearsley 2012) and aluminum foils
(Kearsley 2006, Burchell et al. 2008b, Kearsley 2008, Wozniakiewicz et al. 2009, Kearsley
2009, Price 2010, Wozniakiewicz et al. 2011, Wozniakiewicz et al. 2012a, Wozniakiewicz et
al. 2012b, Wozniakiewicz et al. 2015, Foster et al. 2013, Hörz 2012, Nixon 2012) at the Wild
2 encounter speed. These experiments, in coordination with numerical simulations, allow for
determination of the speed, trajectory and compositional distribution of ejecta on various
materials, which has been important in understanding the origin and distribution of secondary
particles captured in the interstellar collector of Stardust (Burchell et al. 2012, Price 2012).
However, because the acceleration process itself subjects samples to strong shocks
(Bogdanoff, private communication), it is not always possible to unambiguously distinguish
capture effects from acceleration effects (Stodolna 2012b). There are other factors – notably
mineral density and hardness – which are also likely to have influenced the preservation of
different mineral species during the capture within aerogel, and these remain to be fully
understood. Improvements are needed in dust acceleration technology, particularly in
developing the capability of accelerating fragile cometary particles more gently.

A major fraction of the coarse grains (that is, those >2µm in size) may be fragments of
chondrules that bear some chemical and isotopic similarities to those found in chondrites
(Brownlee et al. 2012). Wherever and whenever they formed, it is clear that they formed by
similar high temperature processes that formed chondrules and that they have dramatically
different origins than previously expected for cometary grains (Gainsforth et al 2015).
Although accurate abundance values are difficult to determine in Stardust samples due to the
loss of petrographic context and complexities of fragmentation, the abundance of micro-CAIs
(by number) is on the order of 2% and the abundance of chondrule-like fragments is much
higher (Joswiak et al. 2012). The chondrules and CAIs in Wild 2 provide direct evidence for
profound large scale mixing in the early Solar System, unless there was a high-temperature
process in the outer Solar System that was a source of materials compositionally, isotopically,
and mineralogically similar to those made in the inner Solar System.

Fines

An overriding issue with the Wild 2 samples is the nature of the components that either poorly
survived capture or did not survive at all. This includes micrometer-sized and smaller
components that often stopped in the upper regions of tracks and less robust materials that
were not amenable to capture. Although many Wild 2 submicrometer-sized grains have been
studied, the nature of typical fines remain poorly determined or unknown, mainly due to the
possible severe effects of alteration during the capture in aerogel or on Al foils. While many of
the best studied tracks contain an abundance of well-preserved coarse materials, the contents
of many of the very largest (bulbous) tracks remain enigmatic. Analyses have generally
focused on the well preserved larger components, because they are more amenable to study,
and addressing high-level science questions has been hampered by both the human and
capture selection biases disfavoring fines. For example, isotopically anomalous presolar
grains were expected to be in high abundance in comets prior to the return of the Stardust
samples, but were in fact to be found to be quite rare (Stadermann et al. 2008). Extensive
experimental efforts subsequently indicated that hypervelocity capture on Al foils often
destroys presolar grains leading to anomalously low measured abundances (Floss et al. 2013,
Croat et al. MAPS 2015). This study has not yet been done for particles captured in aerogel.
Similarly, it is not known how the isotopic and chemical properties of small organic-rich grains
collected along tracks have been affected by the capture process (see Objective 4). The
uncertain nature of the fines affects our understanding of the bulk elemental composition of
the comet solids as well as the presence of critically important materials, discussed below,
that may provide direct genetic links to other meteoritic samples.
The relative concentrations of coarse robust and fine or fragile components is an
important measurement that has only been addressed by existing Wild 2 studies in a
preliminary way. The comet is a container of collected nebular materials that were probably
transported to the Jupiter family comet accretion region, although the question of in situ
formation remains open. The fines are an important component that has been difficult to study
and have only been directly studied by a few investigators(e.g., Ogliore et al. 2015). This
“missing component” should be emphasized in future work so that we can better understand
the extent of nebular and Solar System components in comets.

Concentrations of minor phases

Micro-CAIs

A multiyear TEM study of 19 Stardust tracks resulted in the discovery of highly refractory
grains in at least five separate tracks. Mineral assemblages, mineral chemistries and
measured bulk particle compositions (amongst other properties) demonstrated that these
grains are similar to refractory materials in chondrites including fine-grained inclusions, (Krot
et al., 2004; Lin and Kimura, 1998; Simon et al. 2008; Chi et al. 2009; Joswiak et al. 2012) and
Al-rich chondrules (Bridges et al., 2012; Joswiak et al., 2014). Except for the terminal particle
in carrot-shaped track 130, a probable Al-rich chondrule fragment, the refractory grains were
present in Type B/C bulbous tracks in which numerous other rock and mineral fragments were
found, typically including olivines, pyroxenes, sulfides, oxides, and the ubiquitous fine-grained
glassy material formed by impact melting. A major goal is to determine the relationship of
Wild 2 CAIs and meteoritic CAIs, and to determine accurately the modal abundance of
CAIs. (See also Objective 6)

“Kool” grains

A significant number of Stardust tracks contain assemblages consisting of FeO-rich olivines

and Na- and Cr-rich clinopyroxenes (typically augites), sometimes with poorly crystallized
albite or albitic glass with spinel (Joswiak et al. 2009). These assemblages have been named
“Kool” (Kosmochloric high-Ca pyroxene and FeO-rich olivine) grains and are observed in more
than half of all Stardust tracks including all nine bulbous tracks studied by TEM by the
University of Washington group including track 25 (Inti), which contains > 20 CAI fragments.
Kool grains are also observed in chondritic porous IDPs and are relatively common in a giant
cluster interplanetary dust particle believed to have a cometary origin. The textures and
mineral assemblages of Kool grains are suggestive of formation at relatively high
temperatures and indicative of either igneous or metamorphic processes and may have
formed under relatively high ƒO2 conditions. Kool grains appear to be unique to comet Wild 2
samples and CP-IDPs; comparable mineral assemblages and mineral compositions have not
been observed in chondrites. However, FeO-rich olivine andclinopyroxene assemblages in R
chondrites, an oxidized chondrite class, somewhat resemble Kool grains, but have lower Na
and Cr contents than the Kool grains (Joswiak et al. 2009).

The O isotopic composition of a single Kool grain from bulbous track 77 is comparable to
some type II (FeO-rich) chondrule olivines from OC, R, and CR chondrites (Kita et al. 2010,
Isa et al. 2011, Krot et al. 2006, Connolly and Huss 2010). (Tracks are numbered sequentially
in the order in which they are extracted from the aerogel tiles.) No other isotopic
measurements of Kool grains have been made. Because Kool grains are composed of
moderately high temperature minerals, have fine grain sizes, possess approximately
chondritic bulk major element compositions, and are common in cometary materials, these
grains may represent an important contribution to precursor-type materials that formed objects
such as FeO-rich chondrules. One type II microchondrule in Wild 2 shows kosmochloric
enhancement (coupled Na and Cr substitution) possibly reinforcing the link between Kool
grains and chondrule forming processes (Gainsforth 2015). Kool grains would not be
expected to represent the earliest precursor types, however, and likely formed from pre-
existing solids, possibly of nebular origin. Further identification and analysis of Kool
grains by TEM is a high priority, to understand their genesis. The apparent absence of
Kool grains in chondrites may indicate their destruction by parent body processes such as
aqueous alteration.

Micro-chondrules / chondrule fragments

Several tiny igneous rocks from comet Wild 2 have been discovered and analyzed (Matzel et
al. 2010; Joswiak et al., 2012, Ogliore et al. 2012b., Gainsforth et al. 2015, Nakamura et al.
2008a). Morphologically and texturally they are similar to chondrules found in meteorites,
though significantly smaller (Fig. 5). There are also significant differences in the chemistry
and mineralogy of Wild 2 micro-chondrules and meteoritic chondrules: the most common type
of meteoritic chondrule is FeO- and volatile-poor chondrules, called Type I, whereas few
micro-chondrules with such chemistry have been identified in Wild 2 (Joswiak et al., 2012),
although the comet does contain many Fe poor olivines that could be fragments of type I
chondrules. Several examples of FeO-rich, volatile-rich micro-chondrules have been
identified in Wild 2, while meteoritic chondrules with similar properties (of so-called Type II)
are less common. An Al-rich, 16O rich chondrule fragment has also been identified, with
similarities to those present in carbonaceous chondrites (Bridges et al. 2012). Determining
the relationship, if any, between microchondrules found in Wild 2 and chondrules
found in chondrites is a high priority. Do they share a common origin, or are they only
similar because they were once molten?
Fig. 5 Comparison of a typical chondrule with a Stardust “microchondrule”. A) SEM BSE
image of a type II chondrule from the CR2 meteorite GRA 95229, 100 micron scalebar. B)
SEM BSE image of a terminal particle from Stardust named “Cecil,” 2 micron scalebar.

Components found in chondritic porous interplanetary dust particles (CP-IDPs)

An important question is whether the samples returned from Wild 2 are typical of Kuiper Belt
objects. Chondritic porous interplanetary dust particles (CP-IDPs) are commonly thought to
derive from comets, so these serve as a touchstone for comparison with Wild 2. Properties
that suggest CP-IDPs are cometary include their highly fragile porous aggregate structures,
unequilibrated mineral assemblages, high carbon abundance, uncorrelated olivine Fe/Mn
ratios, high presolar grain abundances as well as a number of other characteristics. Thus,
CP-IDPs provide a unique opportunity to compare a likely independent comet sample to Wild
2.

While the comparisons are complicated by selection biases and capture effects, some
statements can be made with confidence. Initial reports (e.g., Ishii et al. 2008) showed strong
differences between Wild 2 samples and CP-IDPs; recent studies are showing affinities (e.g.,
Stodolna et al. 2014). Clarifying the relationship between Wild 2 and CP-IDPs is a major
goal of the next decade of Stardust research, because differences between them may
give information about how and when comets were assembled and how representative
Wild 2 is of other comets. Nesvorny et al. (2010) showed that the distribution of zodiacal
light is consistent with an origin of most interplanetary dust in whole-body break-up of Jupiter-
family comets (JFCs); if this is correct, CP-IDPs sample the entire volumes of JFCs. The
Stardust cometary collector in contrast sampled material from the surface of JFC Wild 2. If
they are different, and if Wild 2 is a typical JFC, then systematic differences may be indicative
of radial heterogeneity in comets, preserving a stratigraphic record of the materials from which
they were assembled, or perhaps reflecting processes altering the surface of comets at least
to some thermal skin depth. The recent observation of apparent depositional layering in JFC
comet 67P/Cheryumov-Gerasimenko (Massironi et al. 2015) may be consistent with this
picture.

The presolar grain abundance in Wild 2 is challenging to measure because of strong capture
effects in the Al foils, but after correction for capture effects, the concentration (~1000 ppm)
appears to be in the middle or upper end of the range observed in CP-IDPs (Floss et al. 2013)
and higher than in chondrites. However, both statistical and systematic uncertainties are
large, so improvement in the accuracy of this measurement is a high priority for future work.

Noble gases have been identified in both IDPs and in Wild 2 samples. We discuss the
question of the origin of noble gases under Objective 8.

Enstatite whiskers, which are thought to be condensation products, are rare components that
are found in CP-IDPs, and were thought to be absent in Wild 2 samples (Ishii et al. 2008a).
An elongated 300-nm long enstatite particle has been observed in Wild 2 (Stodolna et al.
2014), but the Wild 2 enstatite whisker was apparently embedded in a (non-aerogel)
amorphous silicate matrix, unlike enstatite whiskers in CP-IDPs that are unembedded.
It is possible that En whiskers are as abundant in Wild 2 as they are in andydrous IDP.

LIME forsterites (low-iron, manganese-enriched forsterites) with enhanced Mn/Fe ratios (>>
0.5%) are also thought to be condensates. They are commonly found in IDPs and in fact were
first found in IDPs but also exist in chondrites, sometimes as components of amoeboid olivine
aggregates (AOAs). The LIME olivines that have been found in Wild 2 and that have been
analyzed for oxygen isotopic composition have primitive 16O-rich compositions similar to CAIs
, AOAs and the Sun.

GEMS (Glass with Embedded Metal and Sulfides) is an enigmatic sub-micron phase
ubiquitous in CP-IDPs. GEMS are commonly found in anhydrous chondritic-porous
interplanetary dust particles and in some primitive and well-preserved micrometeorites. They
are rarely, if ever, observed in meteorites and are believed to be a cometary component
(Bradley 1994, Bradley et. al 1999, Zolensky et al. 2003). GEMS are easily destroyed by
heating or aqueous alteration. A handful of objects have been discovered in the Stardust
cometary collectors that are generally consistent in composition and morphology with GEMS
in CP-IDPs (e.g., Gainsforth et al. 2016), but the capture processes also produced glass that
mimics GEMS morphology. The hope is that indigenous cometary GEMS can be identified in
the Stardust samples, possibly shielded from impact alteration by a robust terminal particle.
To date, these GEMS-like objects have been found located along aerogel impact tracks and
near terminal particles comprised, in part, by sulfides. This presents a major barrier to ruling
out capture effects as the source of such objects: Stardust speed impacts result in ablation,
abrasion, melting and intimate co-mingling of aerogel and mineral impactors, and those that
involve sulfides generate the nanometer-scale sulfide and metal beads characteristic of CP
IDP GEMS (Ishii et al. 2008a, Abreu et al. 2011, Ishii & Bradley 2015). Thus, it has not yet
been definitively proven that Wild 2 contains GEMS. This is a critical issue because one of
the suggested origins for GEMS is that they are presolar interstellar grains that generally do
not have isotopically anomalous compositions because of homogenization processes that
occur in the interstellar medium (Bradley 1994, Bradley & Ishii 2008, Villalon et. al 2016). It is
possible that Wild 2 contains an abundance of interstellar isotopically normal GEMS that are
unrecognizable because they were small and dissolved into molten silica when they came in
contact with aerogel during capture.

Coarse grains A study of ~50 coarse grains from a single giant CP-IDP consisting of hundreds
of coarse grains ~5 – 40 µm, revealed the presence of four refractory particles (Joswiak and
Brownlee, 2015). Similar to those in Wild 2, the grains consist of moderately refractory
materials and include 3 fine-grained CAIs and a probable amoeboid olivine aggregate. Like
Wild 2, the highest temperature refractory inclusions (e.g., hibonite) in the giant cluster particle
appear to be absent. Two of the refractory inclusions in the giant cluster IDP consist of
individual concentric nodules composed of anorthite/spinel interiors with Al,Ti clinopyroxene
rims with the nodules cemented together in a texture similar to fine-grained refractory
inclusions in chondrites and somewhat akin to Inti, the first CAI found in Wild 2 samples. The
discovery of CAIs in Wild 2 also represents one of the most useful results of the Stardust
Mission: it will permit us to re-examine the existing IDPs and micrometeorites that we have
collected for 40 years and better understand which might originate from comets. When
refractory IDPs were first recognized, 30 years ago (Zolensky, 1987, McKeegan, 1987) they
were assumed to be of asteroidal origin. Now we can look at these samples with new eyes,
leveraging thousands of other samples collected by NASA.
Objective 2: Test the extent of large scale nebular transport and mixing

Question and Objective measurement instrument sample sample

requirements frequency

2 How does material move Concentration of primary analytical TEM,

and evolve in protostellar condensation products (LICE/LIME µXRF/XRD
disks? Determine extent of olivine, enstatite whiskers)
large-scale transport and
mixing

Complementarity between fines and µXRF keystone common

large components

Distribution of olivine Fe content in analytical TEM u/m sections common

microchondrules

Crystalline silicate/amorphous analytical TEM, keystone, u/m common

silicate ratio µXANES sections

Isotopic anomalies, e.g., δ50Ti vs RIMS potted butts rare

δ54Cr, δ50Ti vs δ46Ti, δ62Ni vs δ54Cr
in coarse components

High-precision O-isotope SIMS potted butts common

composition of large silicates

Evolution of carbonaceous material STXM u/m sections rare

Summary of objectives
● Extend high precision O-isotope measurements to micrometer-sized samples
● Improve statistics of O isotope measurements of Wild 2 CAIs and chondrule
fragments, to compare with corresponding meteoritic measurements
● Compare bulk O-isotopic composition of Wild 2 to planetary values
● Determine O-isotopic composition of Wild 2 fines
● Determine abundance of 16O-poor materials like cosmic symplectite in Wild 2
● Determine or constrain oxygen fugacity and formation temperature of Wild 2
rocks
● Compare minor element concentrations in olivines from Wild 2 with olivines
from CP-IDPs and chondrite matrix
● Determine accurately crystalline silicate fraction and variability within Wild 2
samples
● Determine mean and distribution of low-Ca pyroxene to olivine ratio
● Search for isotopic anomalies, e.g., δ50Ti vs δ54Cr, δ50Ti vs δ46Ti, δ62Ni vs
δ54Cr in coarse components
● Compare the bulk composition of fines and coarse-grained component to CI
with sufficient accuracy to test hypothesis of complementarity

Technology advances
 ● Improve sample preparation for high-precision O isotopic composition
measurements
● Improve sample preparation for O isotopic composition measurement of
fines
● Improve ion yield in ion mass spectrometry to allow high-precision O isotope
measurements on ultramicromed slices
● Develop capability of synchrotron hard X-ray transition metal K-edge
spectroscopy with <20 nm spatial resolution
● Develop capability of synchrotron soft X-ray transition metal L-edge
spectroscopy with ~10 nm spatial resolution
● Develop capability of site location through TEM/ALCHEMI
● Improve precision of minor element isotopic composition (Ti, Cr, Ni)
measurements
● Develop high count-rate X-ray detectors with excellent energy resolution (<
10 eV)

In order to explain the presence of refractory and chondrule melt fragments in the Wild 2
samples models of radial drift in the disk plane or above it in disk winds have proved
important. In a model for the solar nebula simulating evolution in surface density of grains due
to diffusion, gas drag, and viscous flows, Ciesla (2007) concluded that outward transport of
high-temperature materials naturally occurs around the midplane of turbulent protoplanetary
disks. In this way material such as micro-chondrules, CAIs or their fragments could potentially
be shifted from the inner Solar System to the comet forming environment 10-30 AU. In support
of this type of model, the coagulation timescale to grow from µm-sized grains to cm-sized
pebbles is expected to be short (<103 a) compared to the radial mixing timescale (>104 a,
Lorek et al 2016).
In contrast to this, Hughes and Armitage (2010) produced 1-D disk models to investigate
radial drift of particles in the protoplanetary disk, and found no model that would sustain
outward transport for large particles (>mm), but smaller particles could still be transported.
Recent observations (Wozniakiewicz et al., 2013 ApJ) of the size distribution of components
of CP-IDPs imply that size-sorting by grain size, composition or density may have occurred
during transport. However, it was found that even the smaller particles (<20 µm) resided in
the outer Solar System for only a short period of time (<106 years). Thus, if the material that
formed Kuiper Belt planetesimals is made of the outwardly transported fine grained chondritic
material (~20 µm), then the Kuiper Belt planetesimals would have had to have rapidly
accreted this material, before it returned to the inner Solar System.. Thus the mechanism of
radial drift seems to remain uncertain, leaving open the question of whether the Wild 2
components formed in the inner or outer Solar System. This is likely to be a topic for much
further study and modeling.
Oxygen isotopic composition of Wild 2 particles

The isotopic composition of oxygen varies throughout the Solar System with bulk planets and
asteroids being depleted by about 6% in the dominant isotope 16O relative to the rare isotopes
17
O and 18O, compared to the Sun, inferred from measurements of solar wind returned by the
Genesis mission (McKeegan et al. 2011). This “planetary” isotope signature is thought to
represent mixing between the 16O-rich bulk solar composition and a 16O-depleted reservoir,
whose nature and origin are a matter of substantial debate. O isotopic variations of different
magnitudes are observed at various spatial scales in extraterrestrial materials and provide a
variety of information about the origin and early evolution of the Solar System. At the smallest
scales, O-rich presolar grains that condensed around stars can be identified by their highly
anomalous isotopic compositions that can differ from Solar System values by orders of
magnitude (Zinner 2014). Percent-level variations are seen at the scale of individual
components of meteorites and IDPs, reflecting both their origins and fractionation occurring
during parent-body processing. For example, CAIs are typically close to the 16O-rich solar
composition, while chondrules, IDPs, and chondrite matrix tend to be closer to the more 16O-
poor planetary signature, and some rare materials (e.g., so-called “cosmic symplectite”) have
been identified in chondrites and IDPs with much more extreme (10-20%) 16O depletions,
perhaps reflecting the primordial 16O-poor nebular reservoir. At the scale of bulk asteroids and
planets, permil differences in O-isotopic compositions are a highly diagnostic classification
tool. Therefore, different questions may be asked based on the level of measurement
precision.

Some key questions regarding O isotopes in Wild 2 samples include:

● What is the abundance of isotopically anomalous presolar grains in comets?
● Do Wild 2 CAIs and chondrule fragments have similar O isotopes to those in
meteorites indicating a genetic relationship?
● Is the bulk O-isotopic composition of Wild 2 solids planetary-like?
● Can the Wild 2 fines’ O-isotopic compositions constrain their origin? (discussed in
Objective 7)
● What is the abundance of 16O-poor materials like cosmic symplectite in Wild 2?
● Are grains found in the Stardust interstellar collector indeed interstellar in origin? This
question is discussed in Objective 9.

As with other Stardust analyses, O-isotopic analyses pose significant technical challenges,
including the difficulty of extracting and mounting small samples for high-precision analysis
and need to distinguish samples or regions of samples that were altered by impact from those
that were not. Nonetheless, a number of O-isotopic studies on Wild 2 samples have been
carried out thus far with increasing sophistication in sample preparation and analytical
methodology, all are based on secondary ion mass spectrometry (SIMS). NanoSIMS
measurements on impact crater residues on Stardust Al foils have been used to identify a few
O-rich presolar grains and constrain their abundance (McKeegan et al. 2006, Stadermann et
al., 2008) though additional searches are desirable. Relatively low-precision (> 10 per mil)
SIMS measurements revealed the first Stardust CAI (Track 25 Inti) to be 16O-rich, similar to
meteoritic CAIs (McKeegan et al. 2006). Higher-precision analyses of silicate grains larger
than a few microns extracted from the aerogel collector, including many chondrule-like
fragments, have found planetary-like signatures similar to those seen in coarse grained
chondritic silicates (Nakashima et al. 2012, Ogliore et al. 2015). But numerous 16O-rich grains
have also been seen including LIME olivines and even a relict forsteritic olivine in a chondrule
fragment (Nakamura et al. 2008) O isotopes in fines have been addressed in two ways.
Ogliore et al (2015) pressed a compressed piece of aerogel containing sub-micron particles
into In and used SIMS imaging methods to determine the isotopic composition of individual
embedded grains. This study found a wider range of O isotopes than has been observed in
other fine-grained planetary materials including chondrite matrices and IDPs (excluding
presolar grains). Snead et al (2015) measured impact residues on Stardust Al foils to avoid
the problem of aerogel contamination and found planetary-like isotope signatures for most, but
possible evidence for a cosmic symplectite-like contribution in one crater.

Additional high-precision O-isotope analyses on Stardust samples are crucial for better
addressing the questions outlined above. Most analyses have been made on “potted butts”
left over from microtoming particles. However, current sample preparation methodologies
(e.g., Westphal et al 2011, Ogliore et al 2015) are for the most part difficult, time-consuming
and often require specialized equipment and training, so simpler methods are highly desirable.

A particularly important goal is to extend the high precision O-isotope measurements

to micrometer-sized samples for the simple reason that the Wild 2 collection contains
only a limited number of larger (terminal grains) but a nearly unlimited number of
smaller fragments that are found in some tracks by the thousands. Measurements of
ultramicrotomed sections, of order 100 nm thick, could also be useful since these are
relatively plentiful, but the amount of material available is insufficient to make high-precision (<
2 per mil at 2σ) oxygen isotopic measurements without improvements in ion yields. Finally,
continued comparison of the aerogel and Al foil samples will also be necessary for extracting
the maximal scientific impact from the collection.

Oxidation state as a probe of mixing and transport

Urey and Craig (1950) were the first to recognize through systematic analysis that the
oxidation state of Fe varies between meteorite groups. Oxygen fugacity may increase with
heliocentric distance of formation, although the relationship is probably not monotonic or
straightforward. Nevertheless, measurement of the oxidation state of Fe and other transition
metals provides constraints on the formation environment of the components of Wild 2, and
any affinities with meteorite groups.

The oxidation state of Fe in Wild 2 is distinct from that of any recognized meteorite family, and
is metal-rich as compared with CP-IDPs (Westphal et al. 2009) although the comet also
contains a major abundance of Fe-rich olivines which must have formed under quite oxidizing
conditions. The difference with CP-IDPs, which appears not to be related to selection biases,
capture effects in aerogel (for Wild 2 samples) or high-speed atmospheric entry (for CP-IDPs),
might be understood if comets are stratigraphically heterogeneous: Stardust sampled only the
near-surface of Wild 2, probably within a thermal skin-depth, while CP-IDPs may sample the
entire volumes of disrupted Jupiter-family comets (Ogliore et al. 2012b, Nesvorny et al. 2010).
This hypothesis may be consistent with the recent observations by the Rosetta mission that
provide evidence for periodic, stratified accretion of comet 67P/Churyumov-Gerasimenko, a
Jupiter-family comet like Wild 2 (Massironi et al. 2015). The hypothesis is also complicated by
mass loss regions on Wild 2 that are well over 100 m deep and the possibility that the entire
comet may have lost hundreds of meters of its surface in the solar-driven sculpting of its
highly complex pitted surface (Brownlee et al. 2004).

In large Wild 2 particles, the distribution of iron content in olivine and the correlations of minor
elements (MnO, CaO, Cr2O3) with olivine iron content seen in Stardust samples are not
observed in any individual meteorite class. The distributions can be reproduced by a mixture
of contributions from known meteorite families (Frank et al. 2014; Brownlee and Joswiak,
2015). However, the apparent overabundance of Type II over Type I micro-chondrules and
chondrule fragments in the Stardust collection suggests that the distribution of Fe-bearing
silicate minerals from the inner Solar System to the outer Solar System may not have been
homogeneous. Assuming that these objects derive from the inner Solar System, these
observations may be used to constrain the timing and selectivity of large-scale transport in the
early Solar System. Studies to date suggest that the compositional dispersions in Wild 2
olivine are similar to olivines in some very primitive CP-IDPs.

A study of Ti valence states using electron energy loss spectroscopy with a transmission
electron microscope showed that variable Ti oxidation states exist in low-Fe augite in nodules
within and between single fine-grained Wild 2 CAIs (Joswiak et al. 2015). This suggests that
the fine-grained cometary CAIs (from Wild 2 and a giant cluster particle) may have moved
between local environments with differing ƒO2 perhaps due to variable dust/gas ratios in a hot
inner Solar System environment prior to transport to the comet-forming region. Similar
variability in Ti oxidation states in low-Fe augite in type A CAIs in chondrites were reported in
CAI interiors and rims (J. Simon et al. 2005; S. Simon et al. 2007). Earlier work on the mineral
osbornite in the Wild 2 CAI Inti showed variable V content within single submicrometer-sized
grains also suggestive of either dynamic nebular conditions or of movement between different
spatial locations during formation (Chi et al. 2009). Interestingly, fO2 values calculated in the
same study from Ti valence states in Inti fassaitic pyroxene, which formed at lower
temperatures and C/O ratios than osbornite, are consistent with formation in conditions like
those for Solar System CAIs.

Ongoing advances in synchrotron X-ray spectroscopy promise to enable better determination

of oxygen fugacity. High spatial resolution hard X-ray microprobes, such as the new hard X-
ray beamline at the National Synchrotron Light Source II, will allow of K-edge spectroscopy of
the transition metals Ti through Fe, allowing for determination of oxygen fugacity over the
entire range of solar-system values. The development of L-edge spectroscopic techniques for
transition metals, currently demonstrated with ~10 nm spatial resolution and the capability of
analyzing ultramicrotomed sections, will require a combination of extensive analyses of
standards combined with ab initio calculations. Site occupancy measurements using
ALCHEMI (Atom Location by CHanneling Enhanced MIcroanalysis) in Transmission Electron
Microscopy may further constrain oxygen fugacity and formation temperature (Gainsforth et al.
2014).

Crystallinity

While crystalline silicates have been observed in circumstellar environments (Molster and
Kemper 2005), it is known that interstellar silicates are almost entirely amorphous (Kemper et
al. (2004, 2005)), so the presence of crystalline silicates in comets implies that a substantial
fraction of interstellar material was subject to high-temperature processes prior to
incorporation into comets. An alternative explanation is that crystalline silicates in comets and
also seen in circumstellar disks forms by low temperature annealing of amorphous materials.
This is clearly not the origin of many Wild 2 crystalline materials, particularly those related to
CAIs and chondrules but it is possible that materials with such origin do exist in the comet but
are hard to positively identify. To the extent that high temperature processes may have been
restricted to the inner Solar System, the fraction of crystalline silicates (Westphal et al. 2009,
Stodolna et al. 2012a) and the abundance of semi-volatile elements, after correction for
aerogel capture effects, may be sensitive quantitative indicators of large-scale nebular mixing,
and may provide constraints that can be compared with models (e.g., Ciesla 2007). Further
studies are needed to improve over the current measurements of the crystalline silicate
fraction, and to determine its variability among Wild 2 samples.

Low-Ca pyroxene/olivine ratio

The ratio of low-Ca pyroxene to olivine varies among meteorite groups (Dobrica et al. 2009),
from ~0.2 for CM meteorites to ~1 for CR meteorites. This number is only approximately
known to be ~1 in Wild 2, but a more accurate measurement of the mean and distribution
of this ratio will help to constrain the mix of materials from which coarse particles in
Wild 2 derive.

Inherited nucleosynthetic anomalies

Different meteorite groups show subtle, systematic isotopic anomalies. For example,
anomalies in 46Ti, 50Ti, 54Cr, and 62Ni have been interpreted as nucleosynthetic anomalies
inherited from distinct Solar System reservoirs (Trinquier et al. 2009). 54Cr is also correlated
with Cu/Yb and Ga/Yb ratios, and varies systematically among carbonaceous chondrites, with
low 54Cr and low Cu/Yb and Ga/Yb for CO meteorites and high values for CI chondrites. The
isotopic anomalies are extremely small, less than 1 part in 105, but a next-generation, high-yield
instrument (e.g., RIMS, Stephan et al. 2016) may be able to approach this precision on ≥20µm particles.
The elemental ratios might be measurable with high energy resolution X-ray detectors such as
micro-calorimeters (Silver et al. 2014): the challenge will not be in measuring the abundances
in the numerators (Cu and Ga) but in the denominator (Yb). Current micro-calorimeters are
limited by low maximum count rates.

Compositional complementarity

If coarse-grained materials in Wild 2 (micro-CAIs, micro-chondrules, etc.) are indeed xenoliths

derived from the inner Solar System, then their composition may not be complementary to that
of the fine-grained material, which, if it is very primitive, may have an elemental composition
similar to that of the Sun. Coarse-grained particles systematically have larger ranges in the
aerogel than fine-grained materials, which tend to stop quickly and so are found in the bulbous
regions of tracks. The separation is not perfect – some fine-grained material that is
mechanically attached to large particles can penetrate to large depths in the aerogel – but
there is sufficient separation that compositional differences can be explored in principle. The
limited synchrotron X-ray analyses (Flynn et al. 2006, Ishii et al. 2008b, Lanzirotti et al.
2008, Schmitz et al. 2009, Tsuchiyama et al. 2009) are not yet sufficient to test this
hypothesis, but future efforts with improved statistics in a coordinated effort may be
able to do so. Mobilization of volatile components in aerogel add to the challenge of this
measurement. On the other hand, if the coarse-grained materials are complementary in
elemental composition to the fines, so that the total composition of Wild 2 is near solar, then
this may be an indication that the micro-chondrules and micro-CAIs formed in situ in the outer
nebula, as suggested by Bridges et al. (2012), or that the fines were transported from the
inner solar system also.
Objective 3: Determine age of cometary material relative to CAIs

Question and Objective measurement instrument sample sample

requirements frequency

26
3 When do comets form in the Al age (Al-Mg systematics) SIMS, RIMS high Al/Mg rare
construction sequence of the plagioclase
Solar System? Determine
relative and absolute age of
cometary materials relative to
CAIs, and timing of large-
scale transport and mixing

53
Mn age (Mn-Cr systematics) SIMS, RIMS high Mn/Cr rare
sphalerite

87
Rb age (Rb-Sr systematics) RIMS high Rb/Sr rare?
phases
(sulfide?)

Summary of objectives
● Search for evidence of live 26Al in large numbers of well-suited Wild 2
samples
● Search for evidence of live 53Mn in large numbers of well-suited Wild 2
samples
● Measure age of Wild 2 samples with long-lived radioisotope systems (e.g.,
Rb-Sr)

Technology advances
● Develop improved synchrotron microprobe search capability for targets for
Al-rich, Mg-poor phases
● Improve methods and standards for Al-Mg and Mn-Cr isotope measurements
in Wild 2 samples
● Develop capability of using long-lived clocks to measure absolute age of
Wild 2 materials

Measurements of short-lived and long-lived radionuclides and their decay products in

meteorites are very useful to determine the chronology of events in the Solar System. The
radioactive parent of short-lived systems used in cosmochemistry, such as 26Al-26Mg and
53
Mn-53Cr, was assumed to be present in the nascent solar nebula at some uniform
abundance. Using a sample that has been suitably dated for both a long-lived and short-lived
system, the short-lived system is “anchored” to the long-lived system and an absolute date
can be inferred. The disadvantage of short-lived systems is that their chronological information
is dependent both on the anchor and the assumption that the initial abundances were the
same everywhere in the young Solar System. The advantage is that certain mineral phases
can concentrate a radioactive parent element with respect to the daughter element. The initial
amount of radioactive parent isotope in a sample (which has long since decayed) is measured
by determining the proportionality constant between the radioactive parent element and the
excess daughter isotope.

26
Al decays to 26Mg with a half-life of 730,000 years. Because of this short half-life, the
presence of 26Al in early solar-system materials can only be inferred through a detection of an
excess of its daughter, 26Mg. A search for excess 26Mg requires samples with very large
Al/Mg ratios, and has been carried out on only four Wild 2 particles so far: two CAI fragments
(“Inti”, Ishii et al. 2010, “Coki”,Matzel et al. 2010a), one chondrule fragment (“Iris”, Ogliore et
al. 2012b) and one ferromagnesian silicate (“Pixie”, Nakashima et al. 2015). No evidence for
live 26Al was found in any of these samples. Coki has mineralogy similar to a type C CAIs in
meteorites, of which half are likely to have been remelted in the chondrule-forming region
(MacPherson 2014). The upper bound of 1×10-5 inferred by Matzel et al. 2010 for the initial
26
Al/27Al ratio in Coki is consistent with the low abundance of 26Al in type C CAIs (Krot et al.
2005). On the other hand, the mineralogy and 16O-rich composition of Inti indicate that this
CAI was not melted during chondrule formation.

A challenge with the Al-Mg dating system is the lack of Al-rich, low-Mg phases, such as
anorthite and hibonite, in Wild 2 samples. Even after years of observation over dozens of
tracks and hundreds of fragments by numerous labs around the world, we still have not found
an ideal fragment for a best-case Al-Mg study. An important future contribution will be to
develop the capability of efficiently searching for Al-rich, Mg-poor phases, probably
using advanced synchrotron X-ray microprobes.

In one model of the early Solar System, the distribution of 26Al was heterogeneous but was
later homogenized in the protoplanetary disk by radial mixing (Krot et al. 2012). Chondrules
would have formed after this homogenization, so dating their formation using the Al-Mg
system is less problematic than dating refractory inclusions like Inti and Coki. The chondrule
fragment Iris (Ogliore et al. 2012b) and the ferromagnesian silicate Pyxie (Nakashima et al.
2015) did not show evidence for the former presence of 26Al (inferred 26Al/27Al< 3-4 × 10-6) .
Assuming 26Al was homogenized at the canonical CAI value of 26Al/27Al = 5 × 10-5 in the
protoplanetary disk soon after the formation of CAIs (MacPherson 2005), these grains must
have formed more than 3 Ma after CAIs. If Pyxie and Iris formed in the inner Solar System,
this implies that large-scale radial transport had to occur very late in the young Solar System
in order to move these particles out to the trans-Neptunian region for incorporation into comet
Wild 2. The formation of Jupiter effectively cuts off in-disk transport of material, so the
presence of these late-forming inner Solar System objects in comet Wild 2 has far-reaching
implications for planet formation (Ogliore et al. 2012b). An additional complication is the
possibility of delayed injection of 26Al in the Solar System. Many Al-rich refractory inclusions in
meteorites show no evidence of radiogenic 26Mg, which has been suggested by some as
indicating not a late formation but rather formation before 26Al was introduced into the inner
nebula (MacPherson 2005, Liu et al 2009; Koop et al 2016). This might happen if 26Al was
injected (e.g., by a supernova) into the collapsing cloud or an already-formed disk where
some 26Al-free refractory objects had already formed.
The 53Mn-53Cr system has been used to measure formation ages of minerals formed by
aqueous alteration on meteorite parent bodies. Secondary minerals like carbonates and
fayalites tend to concentrate Mn and exclude Cr, making them ideal candidates for Mn-Cr
dating assuming that they formed during the lifetime (half-life=3.7 Ma) of 53Mn. One Wild 2
particle, a fayalite-silica intergrowth named Ada, has been measured for the Mn-Cr system by
two different labs (Ogliore et al. 2014, Matzel et al. 2014), but the measured Mn/Cr ratios were
too low to obtain meaningful constraints on the initial 53Mn abundance. However, similar
objects in ordinary chondrites are interpreted to be formed by aqueous alteration. Thus, if Ada
(or similar grains in the Wild 2 collection) formed by a similar process, more robust Mn-Cr
measurements could provide useful constraints on the timing of its formation relative
to alteration timescales in asteroids, if 53Mn in the early Solar System was homogeneous.

Progress in assessing the Al-Mg and Mn-Cr systematics in Wild 2 samples will also benefit
from recent technical advances. For example, a new high-spatial resolution O- ion source for
the NanoSIMS ion microprobe (Matzel et al. 2014) allows measurement of smaller samples
with less contribution from surrounding materials than previously possible. Precise
interpretation of SIMS data for the Mn-Cr system – for meteorite samples as well as for Wild 2
dust – has also been hampered by the difficulty of preparing accurate standards for
determining Mn/Cr elemental ratios. There has been recent progress on this front (e.g. Jilly et
al. 2014), but additional development of improved standards is highly desirable.

Aside from pre-solar grains, which are known to predate the Solar System, the oldest Solar
System materials that have been reliably dated are the CAIs. It is assumed that cometary
solids formed no earlier than this, but actual evidence of this is lacking. Long-lived systems,
such as Pb-Pb dating, are powerful as they provide an absolute age since closure of the
radioisotope system (e.g., Connelly et al. 2012). However, the relatively low cosmic
abundances of Pb, U, and other elements in long-lived systems means samples larger than
~20 mg are required. Samples from comet Wild 2 are too small to be dated using long-lived
systems with current techniques (thermal ionization mass spectrometry and high-resolution
inductively coupled plasma source mass spectrometry). A major goal of current and future
analytical developments is to achieve sufficient precision that long-lived systems in
Wild 2 samples can be made accessible. The newest generation RIMS (resonance
ionization mass spectrometry) instrument, CHILI (Chicago Instrument for Laser Ionization;
Stephan et al., 2016), is designed to determine absolute ages in small grains with
unprecedented precision. Rb-Sr dating should be possible with ≥20 µm particles.
Objective 4: Determine character and origin of organic matter

Question and Objective measurement instrument sample sample

requirements frequency

4 How and where do cometary H, C, N isotopes of organics nanoSIMS shielded rare

organics form? Determine material
origin of organics (possibly behind
terminal
particles),
craters in foils

Composition and structure of Raman, STXM, shielded rare

organics XANES, L2MS, material
GCMS (possibly behind
terminal
particles)

Summary of objectives
● Determine affinities of Wild 2 organics with organics in chondrites and/or
IDPs through analysis of more samples
● Reveal organic reaction networks that may have generated complex organic
matter on the Wild 2 body
● Substantially increase statistics of identification and characterization of
isotopically anomalous organic matter

Technology advances
● Development of new sample-preparation media that do not solubilize
organics or penetrate particles/silica aerogel
● Development of ultra-L2MS for analysis of organics with <5 µm spatial
resolution
● Development of nanoFTIR for analysis of organics with <50 nm spatial
resolution
● Utilization of direct-electron detectors, 40-60 keV electron sources, and
aberration-corrected lenses for high resolution (S)TEM observations at low
beam damage conditions.

Although organic matter is famously known to be abundant in cometary gas and on cometary
surfaces and in coma particles (Goesmann et al. 2015; Greenberg 1998; Lawler and Brownlee
1992), the collection and return of pristine cometary organics was only a secondary goal of the
Stardust mission. Thus, the discovery of carbonaceous matter preserved alongside mineral
grains in captured terminal particles was an unexpected bonus of the mission (Brownlee et al.
2006; Sandford et al. 2006). Cometary carbonaceous material could have been a major
component of the Earth’s original inventory of prebiotic carbon (Pasek and Lauretta 2008).
Three general categories of carbonaceous matter were found in the Stardust aerogel and
foils: (1) soluble compounds present in the coma that infiltrated the aerogel tiles, (2) soluble
and labile organic matter present in coma aggregate grains, and (3) insoluble,
macromolecular organic matter. Cometary soluble compounds impinging on the collector
travelled through the aerogel, ultimately depositing on the Al foil surfaces lining each aerogel
tile. After exposure to hot water extraction and acid vapor hydrolysis, the amino acid glycine
was detected from the side foils, with a “heavy” C isotopic composition, indicating a cometary,
rather than terrestrial, origin (Elsila et al. 2009). α- and β-alanine were also detected, but in
concentrations too low for a robust measurement of their isotopic composition.

Less-soluble, labile organic matter has been observed as extensive organic halos surrounding
some particle capture tracks (Bajt et al. 2009), high concentrations of organics within densified
aerogel without a terminal grain (De Gregorio et al. 2011), and soluble organic components
that have been extracted from fine-grained terminal particles after embedding in epoxy (Cody
et al. 2008a), but no robust characterization of isolated soluble cometary material has been
performed. Cometary insoluble organic matter (IOM), on the other hand, is rare but can be
found both in fine-grained terminal particles, isolated carbonaceous grains embedded in the
walls of bulbous Type B tracks, and as carbonaceous terminal grains. Coherent fragments of
cometary IOM have been identified by TEM and/or STXM in thirteen Stardust particles. In nine
of these cases, the IOM contains a consistent functional group chemistry, dominated by
carboxyl and ketone bonding, with a variable amount of aromatic C=C bonding (e.g., De
Gregorio et al. 2011). This functional group profile is similar to what is observed in IOM from
primitive carbonaceous chondrites (Cody et al. 2008b) and IDPs (Keller et al. 2004), but
without the variability in aromatic carbon abundance observed in the cometary samples. The
lowest aromatic carbon abundance is reported from the terminal particle of Track 57 (“Febo”;
Matrajt et al. 2008) and a bulb wall grain from Track 80 (De Gregorio et al. 2014), while the
highest aromatic carbon abundance was found in carbonaceous nanoglobules (De Gregorio
et al. 2010, 2011). Two of the carbonaceous grains are composed of poorly graphitized
carbon (Matrajt et al. 2013b; De Gregorio et al. 2014), indicating that they were subject to a
heating event, which is unexpected in a cold outer Solar System body. Graphitization could
have occurred by flash heating of cometary organics during hypervelocity capture in aerogel,
but it is also possible that the poorly graphitized carbon formed within the early solar nebula,
prior to accretion onto Wild 2. The functional chemistry of the two remaining verified
carbonaceous grains has not been characterized. Polycyclic Aromatic Hydrocarbons (PAHs)
have also been observed in craters in the Stardust Al foils (Leitner et al. 2008)

Identification and characterization of cometary organic matter is complicated by intrinsic

organic contaminants present in the silica aerogel as well as the potential for destruction or
alteration from flash heating during particle capture (Fries et al. 2009). A significant research
effort was undertaken to characterize possible aerogel contaminants by a variety of
techniques (Sandford et al. 2010). All research programs that target cometary organics must
now take into account these intrinsic contaminants in addition to those introduced by the
terrestrial environment and sample preparation. In addition, the existence of soluble cometary
organics in the Stardust collection requires that some kind of nanoscale imaging (often TEM)
be included in order to distinguish organic-rich aerogel from coherent carbonaceous grains.
An example of this can be seen by comparing the initial preliminary examination results on
cometary organic matter (Sandford et al. 2006) to a later reanalysis of the same samples by
TEM (De Gregorio et al. 2011). The eight carbonaceous grains described in the initial 2006
study showed a wide range of organic chemistry. However, the 2011 reanalysis showed that
only one grain represented verifiable, authentic, unaltered, cometary organic matter (with two
others not available for reanalysis). The apparent wide range of organic chemistry was
reduced to a single functional group profile similar to that seen in chondritic IOM and IDPs (De
Gregorio et al. 2011).

Meteoritic and IDP organics are commonly characterized by searching for isotopic anomalies
in H, N, and, more rarely, C (typically, enrichments in D, 15N, and/or 12C). The origin of these
isotopic signatures is hotly debated but they may indicate an origin in the Sun’s parental
molecular cloud or the outermost regions of the early solar nebula. In any case, the presence
of such anomalies in Wild 2 grains is additional evidence of a cometary origin, similar to the
methodological approach used to verify cometary glycine on Stardust Al foils (Elsila et al.
2009). Isotopic analysis of Wild 2 carbonaceous grains have revealed mostly terrestrial-like
D/H ratios, though a few D-enrichments, with δD up to ~2,000 permil, have been observed
(McKeegan 2006; Matrajt 2008). Nitrogen is mostly terrestrial-like as well, but 15N-rich
carbonaceous grains have been identified both in isolated particles from along bulbous tracks
(McKeegan 2006; De Gregorio 2010) and from shielded fine-grained material in terminal
particles (Matrajt 2008), with δ15N up to ~1200 permil. The range of N isotopic ratios is slightly
more limited than that seen in carbonaceous chondrites and IDPs, whereas the degree of D
enrichment is much more modest. Some carbonaceous meteorite classes (particularly CM,
CV, and CO chondrites) have similar ranges of δ15N and δD values (Alexander et al. 2007).
These meteorites also tend to have fewer “hotspots” with extreme isotopic enrichments, which
may be consistent with the current Wild 2 isotope data. However, these isotopic compositions
may not be so surprising given the fact that so much of the mineral component in the Stardust
collection has inner Solar System origin, and that conditions on the comet are not conducive
to the in situ formation of IOM. Transient aqueous fluids on Wild 2 (Miles and Faillace
2012) could generate the not insignificant amounts of soluble organics that have been
observed so far, making the isolation of soluble organic matter from Stardust terminal
particles and aerogel an essential goal for future work.

A few studies have directly investigated the possible genetic relationship between the
carbonaceous components of Wild 2 particles and those found in primitive carbonaceous
chondrites and IDPs. Using STXM, Wirick et al. (2009) found that chondritic IOM contains
generally more aromatic functionality than that of Wild 2 particles and IDPs. That IOM is
altered by the extraction process is a complication (Flynn et al 2010). In addition, the Wild 2
carbonaceous matter showed a range of functional group diversity that mimicked that
observed in the IDP samples, although, as discussed above, some of this diversity could be
due to contaminants and interactions with silica aerogel during hypervelocity capture.
Comparisons between nanoscale morphology and textures of carbonaceous matter in Wild 2
particles and IDPs and found striking similarities (Matrajt et al. 2013a). Wild 2 carbonaceous
matter typically shows a dense, coherent, “smooth” texture, but globular forms, speckled
“dirty” textures, and lacy or vesicular “spongy” textures have also been observed (Matrajt et al.
2013a, 2013b), all of which are found in IDPs (Matrajt et al. 2012). In contrast, chondritic IOM
tends to be dominated by a porous, mesoparticulate, “fluffy” texture, along with globular forms
and larger “smooth” carbonaceous grains. While these studies suggest a direct link between
IDPs and ejected comet dust, it would be improper to exclude a genetic link with chondritic
IOM, keeping in mind that even the most unaltered, petrologic type 3.0 chondrites have still
experienced some minor amount of parent body heating, pressure, and aqueous fluid flow,
which can change and homogenize the functional group profile of accreted organic matter. In
addition, carbonaceous matter in IDPs is mainly observed as organic coatings on mineral
grains, and only a single example of an organic-coated grain has been reported from the
Stardust collection (Matrajt et al. 2008). The question of potential affinity of Wild 2 organic
content with that found in chondrites or IDPs is certainly ambiguous at present, at least
in terms of the organic content of Wild 2, and the most obvious remedy is to gather
more observations of carbonaceous cometary samples.

A corollary question, which is very much unaddressed, is that if Wild 2 carbonaceous matter is
genetically related to organic matter that is prevalent in IDPs or carbonaceous chondrites, why
do we not find more of it in the Stardust collection? Three factors may be responsible for the
apparent lack of carbonaceous samples. First, carbonaceous matter may simply not be
abundant in the coma dust that was exposed to the Stardust collectors. Polarimetric
observations indicate that the polarization induced by coma dust in the circumnucleus halo
region of Wild 2 is inconsistent with the high refractive indices of solid carbonaceous particles,
and therefore, the abundance of carbonaceous matter in the coma region, from which the
Stardust spacecraft collected material, is naturally low (Zubko et al. 2012). Secondly, flash
heating and explosive volatilization associated with hypervelocity capture into silica aerogel
may have caused a significant sampling bias against carbonaceous matter. Finally there may
be a sample selection bias due to traditional sample preparation techniques that are not
appropriate for analysis of organic samples. All of the carbonaceous Wild 2 samples that have
been verified as cometary (as opposed to contaminants or organic-bearing silica aerogel)
have been prepared by alternative methods--embedding in molten S (e.g., Cody et al. 2008a),
which can be removed by gentle heating, or acrylic, which can be dissolved with chloroform
vapor (e.g., Matrajt et al. 2008). Similarly, placing prepared samples on a C-free substrate for
analysis will greatly increase the ease of discovering cometary carbonaceous matter.
However, it should be noted that for a large survey of 16 Stardust tracks prepared by the
acrylic method, carbonaceous cometary material was only found in five of them.

Technological Advances Related to Organic Analysis

It is not surprising that much of the research on organic matter in Wild 2 has utilized TEM and
STXM techniques, as these two instruments gather information on organic bonding with the
necessary nanoscale resolution to separate authentic cometary material from silica aerogel or
terrestrial contaminants. However, several technological developments within the last ten
years may prove extremely useful for future organic analysis of Stardust samples. New
instrumentation for existing TEM capabilities include direct electron detectors, the availability
of aberration-correcting lens systems, and low-energy 40-60 keV electron sources, which
provide better spatial and spectral resolution while significantly lowering the required electron
dose delivered to the sample. These advancements, then, allow for better analyses with a
marked decrease in beam damage in sensitive organic samples.

A more complete picture of organic matter in Wild 2 can be gained by using additional
spectroscopic techniques, such as laser microprobe mass spectrometry and FTIR, which
could provide complementary information to TEM and STXM analysis. Unfortunately, the
spatial resolution of these alternative techniques is often too poor to be robustly applied to
carbonaceous matter in Stardust samples. However, a unique two-step, laser desorption
laser ionization mass spectrometer (L2MS) has been in continual development since the
Stardust samples were returned (Clemett et al. 2010). The ultra-L2MS can probe both aliphatic
and aromatic bonding with a 10 µm beam spot, and recent improvements to the instrument
have increased its sensitivity by a hundred-fold over previously-published work. Novel,
NASA-funded instrumentation, such as ultra-L2MS, may be promising for revealing the
functional chemistry of soluble cometary organics that have penetrated into the silica aerogel
during capture (Clemett et al. 2014).

The high lateral resolution and chemical specificity provided by NanoFTIR is an emerging
technique that may have applicability to understanding the origin and nature of cometary
organics and the role that aqueous alteration may have played on the cometary parent body.
NASA funding of instrument development has allowed for the recent demonstration that
atomic force microscope (AFM) tip-enhanced spectroscopy can be used to construct infrared
spectral maps of returned samples with <50 nm lateral resolutions. Recently, NanoFTIR
mapping has been used to construct infrared spectral maps of the Wild 2 grain Iris
(Dominguez et al. 2014) and Caligula (Gainsforth et al. 2013b). This work, so far, has shown
that the technique is capable of identifying silicate minerals and mapping out mineralogical
heterogeneity down to 50 nm, and recent work on Murchison indicates that the resolving
power of NanoFTIR could be applied to identification and mapping of important prebiotic
organics (Dominguez et al. 2015).

Commercial NanoFTIR instruments are now starting to become available, and a NanoFTIR
instrument has recently been installed at the Advanced Light Source synchrotron. Looking
towards the future, there are several challenges and opportunities for the application of AFM-
tip enhanced spectroscopy of planetary materials. First, the technique relies on the availability
of IR laser illumination sources, which are expensive and currently limited in wavelength
coverage. However, the availability of IR lasers (e.g., Quantum Cascade Lasers) is
continuously expanding and it seems likely that sources will soon emerge with wavelengths
that allow for the in-situ imaging of additional important functional groups including -OH and
H2O. In addition, coherent THz illumination sources now exist that should provide sensitivity
to astrophysically significant carbon and hydrogen bearing compounds such as polycyclic
aromatic hydrocarbons (PAHs). Efforts to apply sub-micron scale IR and THz spectral
mapping should facilitate further progress in this area and help answer some of the
unresolved questions highlighted in this document.
Objective 5: Search for signs of exposure to liquid water

Question and Objective measurement instrument sample sample

requirements frequency

5 Are products of aqueous Concentration of aqueous alteration analytical TEM, shielded rare
alteration products present in products (phyllosilicates, carbonates, µXRF, material
comets? Establish if cubanite, pentlandite, magnetite) NanoFTIR, (possibly behind
hydration can occur on micro- terminal
cometary parent bodies and if Raman,XRD, particles),
liquid water is present. XANES craters in foils

Summary of objectives
● Determine whether carbonates formed by aqueous processes can be
distinguished from carbonates formed by nebular processes
● Determine the distribution of concentration of carbonate contamination in
aerogel, and in aerogel tiles near Wild 2 tracks with reported carbonates
● Determine whether sulfides formed by aqueous processes can be
distinguished from sulfides formed by nebular or other processes
● Determine whether magnetite formed by aqueous processes can be
distinguished from magnetite formed by nebular or other processes

Technology advances
● Development of FTIR and nanoFTIR for analysis of hydrated phases
● Development of ability to measure H concentration using highly
monochromated TEM/EELS

Phyllosilicates

Classic aqueous alteration products such as phyllosilicates should exist in Wild 2 if alteration
occurred inside the parent body with any substantial frequency. Although they have not been
found, it is possible that they might exist or have existed in the bulbous regions of tracks or in
crater residues. Even if they all melted during capture, their compositions could have left
compositional clues to their former presence (Wozniakiewicz et al. 2015), although the
presence of other minerals in the impacting particles could complicate the search for such
signatures.. Smectite, serpentine, and tochilinite in carbonaceous chondrites and hydrated
IDPs have distinctive elemental abundances that differ from chondritic values. These, along
with other possible clues such as vesicles, could provide evidence for the presence of fine
hydrated matter that melted during capture. Further, large grains (more than ~2 um), if
present, should have had residual TEM-visible structures remaining as shown by Noguchi et
al. (2007) in laboratory-based hypervelocity capture experiments and subsequent TEM,
synchrotron XRD, and FE-SEM analyses. This kind of search could reasonably be done in
sections from bulbous tracks. Other clues may be provided by searching for organic
molecules associated with aqueous alteration, perhaps within the largest terminal particles
that are less susceptible to capture alteration effects. In principle, NanoFTIR (discussed in
more detail under Objective 5) or similar tip-enhanced IR imaging methods may be
used to map surface bound water on samples and to identify products of aqueous
alteration. (Dominguez et al. 2014; Dominguez et al. 2015). Ishii et al. (2016) have
recently demonstrated the capability of detecting H by TEM/EELS, which holds the
promise of measuring this major element at high spatial resolution (several nm) for the
first time in Wild 2 samples.

It is worth also stressing that in all impact experiments using aerogel, we see a wide range of
heating behavior. If phyllosilicates had been a significant phase we would have seen some
tell tale morphologies of heated phyllosilicates, as we see in agglutinates in C chondrites
(Zolensky et al., 2015) and thermally metamorphosed C chondrites (Tonui et al., 2014).

Carbonates

Carbonates are common products of aqueous alteration, so those found in extraterrestrial

samples are commonly taken as a signature of the presence of liquid water. Burchell et al.
(2006) showed that carbonates can survive capture into aerogel. While no large carbonate
grains have yet been identified in returned Wild 2 samples, numerous submicron carbonate
grains, frequently intermixed with other Wild 2 mineral grains, have been found (Flynn et al.
2009), including Mg-Fe-carbonates associated with amorphous silica and iron sulfides
(Mikouchi et al. 2007). Nano-scale carbonates also found associuated with glass and D-rich
IOM in highly primitive GS-IDPs (Busemann et al 2009). A concern until recently has been
that these carbonates may be a contaminant from the aerogel, but a recent search for
carbonates in track-free Stardust flight aerogel by George Flynn and colleagues detected no
carbonate (G. Flynn, private communication). This showed that the aerogel capture medium is
low in carbonates, to the extent that they are homogeneously distributed, so these submicron
carbonates are likely to be indigenous to Wild 2 (Flynn, private communication). . Further,
while Ca carbonate could plausibly be a manufacture contaminant in aerogel, Mg carbonates
are unlikely (Mikouchi et al. 2007). Because carbonates are readily destroyed during aerogel
capture, the implication is that Wild 2 may contain abundant submicrometer-sized carbonates.
Carbonates can also in principle be formed without the presence of liquid water, in gas-phase
reactions in the nebula (Toppani et al. 2005), so the presence of carbonates is not an
unambiguous signature of aqueous alteration. Whether or not carbonates formed by the two
processes can be distinguished by more detailed analyses is not yet known. Further
experimental petrology experiments, to attempt synthesis of carbonates under a suite of
distinct conditions, could elucidate diagnostic criteria for origin locations and processes.

Sulfides

Sulfides in Wild 2 are predominantly pyrrhotite Fe(1-x)S with near troilite FeS composition, but
the existence of a number of unusual sulfides implies diverse origins. Based on a synchrotron
survey of 194 grains in 11 Stardust tracks, the S/Fe ratio is ~0.3 and most of the S is bound
into pyrrhotite/troilite (Westphal et al., 2009). Some pyrrhotites are terminal particles several
micrometers in diameter while others are located within assemblages with igneous textures
(Joswiak et al. 2012, Gainsforth et al. 2013b). In addition, pyrrhotite can occur in association
with pentlandite (FeNi)9S8, sphalerite ZnS, and kamacite FeNi alloy in igneous textures,
though they likely did not form near equilibrium (Joswiak et al. 2012). Other nano-sulfides
have euhedral morphologies and compositions that suggest they formed in a nebular
environment (Stodolna et al. 2014, Gainsforth et al. 2014). The presence of cubanite CuFe2S3
has been interpreted as evidence for aqueous processing (Berger et al. 2011), although it is
known that cubanite can be formed in non-aqueous environments, The presence of
pentlandite, a common component of hydrated IDPs, is consistent with aqueous alteration, but
recently it has been demonstrated that pentlandite can form by other mechanisms (Schrader
et al. 2015). Even if cubanite and pentlandite indicate aqueous activity on Wild 2, Wild-2
sulfides plot within the Fe-Ni-S ternary plot as two modes: either pyrrhotite/troilite, or
pentlandite, with few if any compositions between (Zolensky et al. 2006). This limits the
extent of aqueous processing since by comparison to hydrous IDPs hydrous processes
produce a wide range of pentlandite compositions. It is clear that sulfides trace a very
diverse range of formation and processing environments and perhaps provide some of the
most direct evidence for aqueous alteration within the Stardust sample suite, while at the
same time, limiting the scope of parent body alteration.

Magnetite
The iron oxide magnetite has been identified with synchrotron X-ray diffraction and X-ray
Absorption Near-Edge Spectroscopy (Fe K XANES) in Stardust samples (Changela et al.
2012, Bridges et al. 2015). One terminal particle from track 183 was found to consist mainly
of Cr-rich magnetite nanoparticles (De Gregorio et al. submitted). These detections of
magnetite are significant because in carbonaceous chondrites Ti-free magnetite is a typical
product of hydrous alteration of ferromagnesian silicates like olivine and pyroxene. The origin
of magnetite in the matrix of carbonaceous chondrites through reaction of ferromagnesian
silicates with parent body water was established by Kerridge et al. (1979) in a study of CI
chondrites and provides a clue for ongoing research that materials in Wild 2 did experience
significant aqueous alteration. On the other hand, high-temperature heating of chondritic
metal, perhaps during nebular shocks or chondrule-forming events, can also produce
magnetite and chromite with trace metal abundances proportional to that of the original metal
(Lauretta and Schmidt 2009), and it is possible that magnetite could even form as a primary
nebular condensate within specific P-T-fO2 conditions. More detailed observation of Wild 2
magnetite is clearly necessary in order to reliably assess their origin.
Fig. 6. Two magnetite terminal particles in Stardust track 187, identified by XRD at the
Diamond synchrotron (Bridges et al. 2015).
Objective 6: Determine formation conditions of micro-chondrule/chondrules, micro-
CAIs, and metals

Question and Objective measurement instrument sample sample

requirements frequency

6 How and where do cometary Element partition in SEM, analytical microchondrule common
rocks form? Determine micro- microchondrules, and micro-CAI TEM s
chondrule and micro-CAI volatile element concentration
formation conditions

Ni et al. trace siderophile siderophile-free large metal rare

concentrations in metal grains sample particles (e.g.,
preparation, LA- Simeio)
ICP-MS

Summary of objectives
● Substantially improve statistics of detailed elemental, mineralogical, and
isotopic analyses of microchondrules/chondrules
● Substantially improve statistics of detailed elemental, mineralogical, and
trace-element analyses of microCAIs
● Substantially improve statistics of detailed elemental, mineralogical, and
trace-element analyses of metals

Technology advances
● Development of W-, Pt-, Au-, Ga-free FIB techniques for sample preparation
of metal particles
● Develop efficient search techniques for micro-CAIs using synchrotron X-ray
microprobes

Micro-chondrule/chondrules

An open question is whether micro-chondrules in Wild 2 share a common formation

mechanism with chondrules in meteorites, or whether the only feature they share is the fact
that they were once molten. The distribution of cations between phases in these objects may
constrain their formation environment. In three micro-chondrules that have been studied in
this way, cooling times and formation environments appear to have been similar to formation
conditions of chondrules (Gainsforth et al. 2015). Another area of active investigation is
whether determination of crystal site occupancy of cations through ALCHEMI may constrain
formation conditions. Many more analyses, including oxygen isotope studies, are
needed to assess the range of formation conditions.

Micro-CAIs
Based on textures, mineralogy and mineral chemistries, the Wild 2 fine-grained refractory
particles appear to be most closely related to fine-grained inclusions which are commonly
found in CV3 and more rarely in CO and CR chondrites and the primitive ungrouped
carbonaceous chondrite Acfer 094. Particle sizes of the Wild 2 refractory inclusions range
from ~1 to 20 µm, the latter size representing the terminal particle from track 25 Inti. These
sizes likely represent lower bounds as fragments may have disaggregated during capture. In
general, refractory grains were found in about one-fifth of all tracks and in nearly 50% of all
bulbous tracks. Considering all studied large fragments from 19 tracks, a rough estimate
indicates that ~2% of Wild 2 fragments are CAIs. The Wild 2 CAI population appears to lack
the most refractory CAI types such as Type A, hibonite-spinel and grossite-bearing varieties.
Nor have the highest temperature minerals – corundum Al2O3,
hibonite (Ca,Ce)(Al,Ti,Mg)12O19, grossite CaAl4O7 – been found in Stardust tracks. The high
temperature mineral perovskite was observed as a rare phase in the terminal particle Inti from
track 25 but has not been observed elsewhere. At present, the reason for this segregation is
unclear. Resolving this uncertainty is a high priority for future research. Key will be to
identify more micro-CAIs for study; high-resolution synchrotron X-ray microprobes
may be particularly useful for this project.

Cometary metals

Wild 2 contains large metal particles, with diverse chemical compositions. One particle,
Simeio, showed an unusual composition, with a very low Ni/Fe ratio and a trace element
pattern most consistent with ureilitic metal (Humayun et al. 2015). Metal grains have also
been seen in numerous olivine grains and most spectacularly in the 40 µm chondrule,
Gozensama, the first chondrule fragment identified in Wild 2 (Nakamura et al. 2008a).
Additional metal particles have been identified by synchrotron XRF and XANES analysis, but
more particles will be needed to determine distributions for comparison with meteoritic metals.
Particle handling and sample preparation are particularly challenging for metal particles.
Sample preparation techniques are currently in development for this purpose that do
not contaminate samples with critical elements (Pt, W, Ga) (Burnett et al. 2016).
Objective 7: Determine origin of fines

Question and Objective measurement instrument sample sample

requirements frequency

7 How much interstellar Mean and dispersion of elemental µXRF, SEM/EDX keystone, common
matter is preserved in composition of fines craters in foils
comets? Determine origin of
fines

O-isotopic composition of fines SIMS dissected common

keystone,
craters in foils

Presolar grain concentration in fines nanoSIMS keystone, rare

craters in foils

Isotopic anomalies, e.g., δ50Ti vs RIMS shielded rare

δ54Cr, δ50Ti vs δ46Ti, δ62Ni vs δ54Cr material
in fines (possibly behind
terminal
particles),
craters in foils

Summary of objectives
● Substantially improve statistics of oxygen-isotopic composition
measurements of fines
● Determine bulk elemental and isotopic composition of fines for comparison
with CI abundances

Technology advances
● Develop technique for laboratory hypervelocity capture experiments using
fines, with gentle acceleration

The fines (submicron components) are very important because they are a major fraction and
perhaps the dominant fraction of the non-ice component mass of Wild 2. They will also take
on increasing importance to future studies of Wild 2 samples because the collection contains
nearly an unlimited number of grains smaller than a few microns. They have not been
adequately studied or even adequately searched because they were not “low hanging fruit”.
They are difficult to study because they are small and they were commonly altered by capture
heating and contact with molten silica. It is critical that work on these small components
adequately distinguishes primary properties with those altered by capture. Most of the
materials preserved as coarser grains have also been seen in fines, but it is possible that
there were some fine components that did not survive capture. One possible way to make
progress on the fines is to study the very smallest bulbous tracks (< 50 µm long) where
thermal heating may have been significantly less than for the larger ones.
Because they contain relatively large phases, the largest Stardust particles are the easiest to
extract and prepare, are the best-preserved, and contain relatively large phases, the largest
particles have been the subject of the most intense investigation. However, there are
indications that the fine-grained components of Wild 2 particles could be systematically
different from the coarse-grained components. This may not be unexpected, if the coarse-
grained components are “xenoliths” derived from the inner solar-system, and the fine-grained
components are the relatively unprocessed solids that were present in the Kuiper Belt at the
time of comet formation. The strongest evidence for such a systematic difference between
coarse-grained and fine-grained material comes from oxygen isotopes, in which fine-grained
material in one track shows a very large spread consistent with mixing with a very 16O-poor
component like cosmic symplectite (Ogliore et al. 2015). If confirmed through more
analyses, this would lend strong evidence for a two-reservoir model to explain one of
the key unsolved problems in planetary science: what is the origin of the pattern of
oxygen isotopic composition of the Solar System, in the three-isotope oxygen
diagram?

The best opportunity for study of unaltered fine-grained material may be in a few rare cases in
which it has been protected from damage during aerogel capture by proximity to a large,
mechanically robust particle. So far two such cases, Febo and Andromeda, have been found,
and in both cases, a field of fine-grained material appears on the downstream side of a large
sulfide particle, although the pristinity of the fine-grained material related to Febo has been
questioned (Ishii et al. 2015). Fig. 5 shows an SEM view of Andromeda with a large sulfide
on the left and the FGM on the right. Technique development is needed to identify such
assemblages before embedding in epoxy or acrylic and ultramicrotomy, to avoid
alteration, mobilization, and contamination of organics. Although materials captured in
aluminum foils are generally more severely altered than in aerogel, these materials may also
be a resource for study of fine-grained materials. It is known that a fraction of submicron pre-
solar grains survive capture in aluminum foils at ~6 km/sec capture speed. (Haas et al. 2016)
Figure 5: SEM image of the terminal particle named Andromeda. The large sulfide on the left
may have partially shielded fine-grained materials during capture in aerogel, including
crystalline and amorphous silicates and sulfides.
Objective 8: Determine pre-accretionary space exposure, shock history, and ion
irradiation histories

Question and Objective measurement instrument sample sample

requirements frequency

8 What is the history of Solar flare track concentration in TEM not yet detected rare
cometary materials before silicates
comet formation? Determine
pre-accretionary space
exposure, shock history, ion
irradiation, and thermal
metamorphism

Noble gas concentration, noble gas keystones unknown

composition, and carrier spectrometry

Concentration of shocked phases µXRD, analytical keystones, u/m common

TEM, SXRD sections

Concentration of products of analytical TEM u/m sections rare

secondary thermal processing

Cosmogenic nuclides AMS

Summary of objectives
● Substantially improve statistics in search for solar-flare tracks, and
determine whether tracks survive aerogel capture.
● Substantially improve statistics in search for shocked phases
● Address reasons for current variability of noble gas concentrations and
compositions in Wild 2 cometary materials and capture media, through
expanded studies in multiple laboratories
● Determine whether the mineralogical criteria for identification of thermal
metamorphism, which has been formulated principally for ordinary chondrites
(OCs) and carbonaceous chondrites (CCs), can be applied to fine-grained
materials in comets.

Technology advances
● Develop technique for laboratory hypervelocity capture experiments with
gentle acceleration to determine whether aerogel capture can induce shock
effects in minerals

Space exposure

A determination of the space exposure time of the components of Wild 2 would be of great
interest in the study of transport in the disk. To date, no solar flare tracks have been found
in any of the Wild 2 particles, suggesting that they were never exposed to solar flare
particles, but no systematic search has yet been done. If tracks were not lost during
capture, this suggests that all transport occurred when the disk retained gas that blocked
energetic solar particles. Particles that were transported to the inner edge of the nebular disk
might have been propelled from the innermost regions of the disk where they could have been
exposed to high radiation environments, different oxidation states, and accretion of exotic
components. An example of possible exotic effects close to the Sun might explain how
nanophase osbornite TiN, Ti,V nitrides, and Platinum Group Elements nuggets became
incorporated inside some of the Wild 2 CAIs. Osbornite condensation is predicted to only
occur from gas with a C/O about twice the solar ratio.

Shock

Tomeoka et al. (2008), Jacob et al. (2009), Joswiak et al. (2012), and Gainsforth et al. (2015)
reported shock effects in olivines and pyroxenes, which could be interpreted as evidence for
mild shock. However, Stodolna et al. (2012b) showed that shock up to 1.5 GPa is produced
by the combination of light gas gun, aerogel capture, and ultramicrotomy. Therefore it is not
clear to what extent shock is present or absent in the comet without better characterizing the
cause of the shock effects observed in the Stardust samples. A high priority is to confirm (or
not) that some Wild 2 samples have undergone shock processes, because this has major
implications for comet assembly or possibly cometary fragmentation as suggested by Farinella
and Davis (1996) and Davis and Farinella (1997) . This will require much more extensive
TEM analyses of laboratory materials shot into aerogel as well as Wild 2 cometary
samples, and possibly improvements in laboratory hypervelocity capture experiments.

Noble gases

The noble gas concentration measured in a few Wild 2 particles is extremely high, higher than
found in IDPs, but many Wild 2 particles are noble gas free (Marty et al. 2008, Palma et al.
2013). These high concentrations may be due to exposure of particles to solar energetic
particles during the Sun’s active phase, before incorporation into the comet. Strikingly high
Ne concentrations are present in the track 41 particles, comparable to or exceeding those
implanted into lunar fines and many IDPs by solar wind ions and suggesting gas acquisition
by ion irradiation, in this case by a compositionally non-solar ion flux, for the track carrier
grains (Marty et al., 2008). The noble gas patterns measured so far show no coherent
pattern, so the noble gas carrier or carriers are unknown. To further complicate matters,
some aerogel sections that are apparently track-free show the unexpected presence of noble
gases, perhaps derived from nearby tracks (Palma et al. 2012).

The principal finding of these studies is the firm identification of the Q-Ne isotopic signature in
Wild 2 coma grains, and the implication of this observation that Q-gases existed in the Solar
System early enough in its history to be incorporated into comets. Apart from that, there are
two outstanding issues to be addressed in future Stardust measurements. Noble gases
measured in the subsurface block samples from cell C2044 are isotopically extremely variable
and show no coherent pattern, nor are they associated with any detectable carrier grains.
Moreover the locations of these noble gas enclaves in C2044 are several millimeters removed
from both the cell surface and the axis of track 41, well beyond the penetration range of solar
wind ions, and there are no visible aerogel damage tracks connecting them to either the
surface or the track. Even if some mechanism could be invoked to eject trackless and
unobserved fragments from the track bulb wall to distant block aerogel positions, the wide
compositional variability of the He and Ne in these samples argues against their origin from
the isotopically Q-like track 41 impactor. Further analyses are needed to elucidate the
origin of the variability.

Thermal metamorphism

The low-Ca pyroxene/olivine ratio and their compositions are also sensitive indicators of the
physico-chemical conditions of grain formation, permitting elucidation of cooling rate, degree
of aqueous alteration, and thermal metamorphism. Olivine and low-Ca pyroxene minor
element compositions particularly provide evidence for thermal metamorphism having
occurred (Frank et al. 2014). However, an open question is whether the mineralogical
criteria for this, which has been formulated principally for ordinary chondrites (OCs)
and Carbonaceous Chondrites (CCs), can be applied to fine-grained materials in
comets. Future TEM work on OC and CC matrices could settle this issue.

Objective 9: Determine flux, size and velocity distribution, composition, and structure
of local interstellar dust in the inner Solar System

Question and Objective measurement instrument sample sample

requirements frequency

9 What is the nature of local Track density, elemental optical picokeystones, ultrarare
interstellar dust? Determine composition, min/pet and isotopic microscopy, foils on
flux, size and velocity composition of IS candidates SEM/EDX, stretchers, O
distribution, composition and massively isotope sample
structure of interstellar dust in distributed prep for tracks
the inner Solar System search, STXM, in development
µXRF/XRD,
nanoSIMS,
SIMS, RIMS

Summary of objectives
● Substantially improve statistics of identified interstellar dust candidates in
aerogel
● Substantially improve statistics of identified interstellar dust candidates in
aluminum foils
● Determine mass, mineralogical and elemental composition of interstellar
candidates in aerogel
 ● Determine mass, mineralogical and elemental composition of interstellar
candidates in foils
● Measure oxygen isotopic abundances in ISD candidates in aerogel
● Measure oxygen isotopic abundances in ISD candidates in Al foils

Technology advances
● Development ultra-low risk technique for sample preparation for oxygen
isotopic composition measurement of ISD candidates in aerogel
● Improve precision of O-isotopic composition measurements of residues in
ISD craters in foils
● Develop capability of isotopic measurement of minor and trace elements in
ISD candidates

In addition to the goal of capturing and returning of cometary materials from the Jupiter-family
comet Wild 2, Stardust had the goal of capturing and returning the first solid samples from the
local interstellar medium. To that end, a separate collector was exposed to the interstellar
dust stream for ~200 days in two episodes, before the encounter with comet Wild 2. This is
the smallest curated collection in the JSC curatorial facility by orders of magnitude. Despite
their size, these samples are extraordinarily valuable both because of their extreme rarity and
because they are likely to be the first solid local interstellar materials ever returned to
terrestrial laboratories for study.

A consortium (the Interstellar Preliminary Examination, ISPE) (Westphal et al., 2014b) was
formed to identify and analyze candidate interstellar dust impacts in the aerogel tiles
(Westphal et al., 2014a, Frank et al. 2013, Bechtel et al. 2013, Butterworth et al. 2014,
Brenker et al., 2013, Simionovici et al. 2014, Flynn et al. 2014, Gainsforth et al. 2014,
Postberg et al. 2014, Sterken et al. 2014) and aluminum foils (Stroud et al. 2014). This project
resulted in the discovery of seven particles of likely interstellar origin, and also provided an
upper limit on the flux of interstellar dust in the Solar System that is substantially lower than
was expected based on the observations of interstellar dust by the Ulysses and Galileo
spacecraft (Westphal et al. 2014c). Since the end of the ISPE, scanning and identification of
tracks in aerogel and craters in foils has slowed, principally because of limited resources at
the curation facility at Johnson Space Center. Nevertheless, impact identification is
continuing, through the Stardust@home distributed search (Westphal et al. 2014a) and,
recently, through a parallel effort called foils@home to identify impacts in foils (Stroud et al.
2016). A complete identification of all impacts will require several more years. Despite the
effort, the project is clearly scientifically compelling: this collection has the potential to contain
the first interstellar dust particles ever identified and analyzed in terrestrial laboratories. (It is
important to draw a distinction between interstellar dust -- tiny particles currently residing in
the local interstellar medium, probably no more than a few hundred Ma old -- and circumstellar
dust -- condensates from circumstellar outflows, which are probably a small component of the
interstellar dust. The only samples of circumstellar dust unambiguously recognized so far are
the so-called presolar grains -- ancient circumstellar grains that pre-date the Solar System and
became incorporated into planetary materials.)

The evidence for interstellar origin for the seven candidates identified so far is strong
(Westphal et al. 2014c) but circumstantial. Recently Silsbee and Draine showed that two of
the largest particles, Orion and Hylabrook, require special optical properties to be consistent
with their apparently low capture speed in aerogel (Silsbee and Draine 2016). The mean
isotopic composition of oxygen in the interstellar medium differs significantly from that of the
solar system. A robust test of interstellar origin requires a measurement of oxygen
isotopic composition of these candidates and others that are identified in the future
with sufficient precision and accuracy that they can be distinguished from particles of
solar-system origin. But we should note that IS grains could be isotopically solar within
measurement precision. Measurements can be carried out now in particles captured in the
aluminum foils of the collector, but the error bars are not sufficiently small to determine their
origins. For the particles in aerogel, the challenge is different: the measurement requires
that the particles be exposed, but no reliable technique exists yet for preparing ~1µm
particles captured in aerogel for isotopic analysis in a SIMS instrument (Westphal et al.
2016b).

The CHILI instrument (Stephan et al, 2016) is ideally suited for analyses of ISD particles,
because of its extraordinarily efficient use of the samples. Work is ongoing to develop
sample preparation techniques for ISD analysis with CHILI. The Al-Mg chronometer is a
likely target for technique development.

SUMMARY

The comet Wild 2 samples returned by Stardust have provided information on the early Solar
System that could not have been known without actual proven comet samples in the
laboratory. The low abundance of isotopically anomalous grains, and the presence of CAIs
and abundant chondrule fragments has profoundly influenced the understanding of the
formation of comets and icy planetesimals and has provided evidence of large scale
movement of common asteroid building materials across the Solar System. While the
program has greatly exceeded common expectations for the low cost Discovery 4 mission,
there is much more that needs to be done. The next comet sample return is well off in the
future and the Wild 2 material will remain a unique resource for years to come. The use of
refined handling and analytical methods, researchers that are well experienced with dealing
with these small complex samples, the accumulated knowledge needed to recognize
alteration from high-speed capture and the accumulated insight into important issues that can
be studied with these samples: all provide an excellent base from which to launch future
studies. To optimize the science return from the Stardust mission, these studies should be
coordinated in ways that maximize the science return from each track and crater because
each particle contains information rich-materials with very important stories to tell. The finding
of CAIs, 16O rich phases, an excellently preserved isotopically anomalous pre-solar SiC grain,
and good candidates for dating using short-lived isotopes were all done on minor components
of capture tracks that could easily have been overlooked, lost, or destroyed in the samples
studied during the early years of Wild 2 studies. A major lesson from the comparison of the
organized consortium-based approach applied to the Interstellar side of the collector with the
more traditional approach to analyses of the comet side is that coordinated approaches with
planned focus are the most productive and the best use of these precious samples. Well-
coordinated future studies should be able to answer some of the most burning questions on
Wild 2 materials such as determining if the Wild-2 chondrule-like and CAI-like components are
derived from the same source regions as their chondrite counterparts or if they were just
made by similar nebular high temperature processes and may have come from different
locales plausibly at different times.

A major point not discussed in this paper is the question of how representative Wild 2 is of
Jupiter Family comets. We know that volatiles vary from comet to comet but what about the
rocky materials that actually dominate the mass of most comets? If all rocky materials were
transported to the comet accretion region, then they might have similar mixes of materials. If
comets accreted over an extended period of time, there might be comets that contain different
mixes of materials transported from different regions or different times. One way to address
this is to use Wild 2 to identify IDPs or even meteorites that come from other comets. This is
a bit of a bootstrap but it might be done simply by comparing the compositional dispersion of
accreted materials. One interpretation of the broad range of materials in Wild 2 is due to its
formation by scavenging material from dispersed environments while chondrite classes are
distinctive because they contain large amounts of regionally produced components.

Acknowledgments

This paper is the product of a workshop that was held near the UC Berkeley campus on July
26-27, 2015, just prior to the 78th annual meeting of the Meteoritical Society. The workshop
was supported by NASA and sponsored by the Curation and Planning Team for
Extraterrestrial Materials (CAPTEM), a NASA advisory committee
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Glossary of Experimental Techniques

Acronym Technique Incident particles Signal Science Goal

ALCHEMI Atom Location by CHanneling Enhanced Electrons Electrons Site occupancies

MIcroanalysis

AMS Accelerator Mass Spectrometry Isotopic

composition

APT Atom Probe Tomography photons Ions Nano morphology,

element
abundances and
isotopic ratios

EDX or EDS Energy-dispersive X-ray Spectroscopy Electrons, ions, or X-ray photons Sample
X-ray photons composition
(similar to XRF)

EELS Electron Energy-Loss Spectroscopy Electrons Electrons Chemical

environment of a
specific element
(similar to XANES)

EPMA Electron Probe Microanalysis Electrons Electrons + X-ray Sub-micron

photons morphology and
composition

FIB Focussed Ion Beam Milling Ions Electrons and ions Sample
Preparation

FTIR Fourier Transform Infrared Spectroscopy Infrared photons Infrared photons Bonds

HIM Helium Ion Microscopy Ions Electrons and ions Particle structure

HRTEM High-resolution Transmission Electron Electrons Electrons Crystal structure

Microscopy and atomic scale
defects

L2MS Two-Step Laser Desorption Mass photons Ions Trace element

Spectrometry abundances and
isotopic ratios

LA-ICP-MS Laser Ablation — Inductively Coupled photons Ions Trace element

Plasma Mass Spectroscopy abundances and
isotopic ratios

LGCMS Liquid Gas Chromatograph Mass Composition of

Spectroscopy organics

nanoFTIR nanometer resolution FTIR Infrared photons Infrared photons Bonds

nanoSIMS nanometer resolution Secondary Ion Ions Ions Isotopic ratios of

Mass Spectrometry elements

noble gas Noble Gas Mass Spectrometry Noble gas

analysis concentration and
isotopic ratios
pSTXM Ptychography/STXM X-ray photons X-ray photons Nanoscale
morphology and
chemistry (similar
to XANES)

RIMS Resonance Ionization Mass Ions or photons Ions Isotopic ratios of

Spectrometry elements

SEM/EDX Scanning Electron Microscope with Electrons Electrons + X-ray Sub-micron

Energy Dispersive X-ray Spectroscopy photons morphology and
composition

SIMS Secondary Ion Mass Spectrometry Ions Ions Isotopic ratios of

elements

(S)TEM/EDS (Scanning) Transmission Electron Electrons Electrons + X-ray Nanoscale

Microscopy with Energy Dispersive X-ray photons morphology and
Spectroscopy composition

SXRD Synchrotron-based X-ray Diffraction X-ray photons X-ray photons Crystal structure

SXRF Synchrotron-based X-ray Fluorescence X-ray photons X-ray photons Sample

Spectroscopy composition
(similar to EDS)

TOF-SIMS Time-of-Flight Secondary Ion Mass Ions Ions Elemental and

Spectrometry isotopic ratios,
organics

XANES X-ray Absorption Near-Edge X-ray photons X-ray photons Chemical

Spectroscopy environment of a
specific element
(similar to EELS)