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Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

Flynn, G. J.↗

Chemical characterization of seven Large Area Collector particles by SXRF

Optical microscopy and synchrotron X-ray fluorescence (SXRF) are used to analyze the chemical composition of seven dark-appearing cosmic-dust particles obtained in the stratosphere during NASA Johnson Large Area Collector flights. The experimental setup and procedures are outlined, and the results are presented in extensive tables. Three of the particles had abundances similar to those of chondrites (except for low Ca values in one particle); two had a metallic appearance and spectra dominated by Fe and Zn; one contained Cu and Cr plus small amounts of Fe and Zn; and one had igneous-type abundances of minor and trace elements while containing all of the elements seen in chondritic particles, suggesting it may be of extraterrestrial origin.

Flynn, G. J.↗

Petrogenesis of the Zagami meteorite - Inferences from synchrotron X-ray (SXRF) microprobe and electron microprobe analyses of pyroxenes

Major and minor element abundances in pyroxene, principally pigeonite, from Zagami meteorite samples were determined by electron microprobe; abundances of trace elements Ni, Cu, Zn, and Ga were obtained by synchrotron X-ray (SXRF) microprobe. Abundances of Ni and Cr in the magnesian zones and cores are partially decoupled from abundances of other compatible (Mg) and incompatible (Fe,Ti) elements. The textures, chemical zoning, and element decouplings in the pigeonites are consistent with igneous crystal growth at moderate cooling rates, not isothermally or near equilibrium. From element partitioning and mass balance, Zagami is estimated to contain 20 +/- 5 percent or less cumulus pyroxene (half augite and half pigeonite), half the proportion suggested by equilibrium distribution of Fe/Mg between pigeonite and melt. This inconsistency may be resolved if all pigeonite/melt element partitioning was affected by the rapid growth of the pigeonites. The inference that the pyroxene zoning patterns reflect only magmatic events is consistent with an igneous age of 180 m.y. for Zagami.

Treiman, A. H.↗

SXRF determination of trace elements in chondrule rims in the unequilibrated CO3 chondrite, ALH A77307

The concentrations of Ni, Cu, Zn, Ga, Ge, and Se in five chondrule rims in the CO3 chondrite ALH A77307 (3.0) using the synchrotron x-ray fluorescence (SXRF) microprobe at Brookhaven National Laboratory were determined. The data show that the trace element chemistry of rims on different chondrules is remarkably similar, consistent with data obtained for the major elements by electron microprobe. These results support the idea that rims are not genetically related to individual chondrules, but all sampled the same reservoir of homogeneously mixed dust. Of the trace elements analyzed Zn and Ga show depletions relative to CI chondrite values, but in comparison with bulk CO chondrites all the elements are enriched by approximately 1.5 to 3.5 x CO. The high concentrations of the highly volatile elements Se and Ga and moderately volatile Zn (1.5 to 2 x CO) in rims show that matrix is the major reservoir of volatile elements in ALH A77307.

Brearley, Adrian J.↗

Non-destructive trace element microanalysis of as-received cometary nucleus samples using synchrotron x ray fluorescence

The Synchrotron X ray Fluorescence (SXRF) microprobe at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory, will be an excellent instrument for non-destructive trace element analyses of cometary nucleus samples. Trace element analyses of as-received cometary nucleus material will also be possible with this technique. Bulk analysis of relatively volatile elements will be important in establishing comet formation conditions. However, as demonstrated for meteorites, microanalyses of individual phases in their petrographic context are crucial in defining the histories of particular components in unequilibrated specimens. Perhaps most informative in comparing cometary material with meteorites will be the halogens and trace metals. In-situ, high spatial resolution microanalyses will be essential in establishing host phases for these elements and identifying terrestrial (collection/processing) overprints. The present SXRF microprobe is a simple, yet powerful, instrument in which specimens are excited with filtered, continuum synchrotron radiation from a bending magnet on a 2.5 GeV electron storage ring. A refrigerated cell will be constructed to permit analyses at low temperatures. The cell will consist essentially of an air tight housing with a cold stage. Kapton windows will be used to allow the incident synchrotron beam to enter the cell and fluorescent x rays to exit it. The cell will be either under vacuum or continuous purge by ultrapure helium during analyses. Several other improvements of the NSLS microprobe will be made prior to the cometary nucleus sample return mission that will greatly enhance the sensitivity of the technique.

Sutton, S. R.↗

Trace element content of chondritic cosmic dust: Volatile enrichments, thermal alterations, and the possibility of contamination

Trace element abundances in 51 chondritic Interplanetary Dust Particles (IDP's) were measured by Synchrotron X-Ray Fluorescence (SXRF). The data allow us to determine an average composition of chondritic IDP's and to examine the questions of volatile loss during the heating pulse experienced on atmospheric entry and possible element addition due to contamination during atmospheric entry, stratospheric residence, and curation.

Flynn, G. J.↗

Removal of carbonaceous contaminants from silica aerogel

Capture of micrometeorite material from low Earth orbit or dust grains around active comets for return to terrestrial laboratories, capable of practicing the most up to date techniques of chemical isotopic and mineralogical analysis, will greatly enhance our knowledge of primitive material in the solar system. The next generation of space launched cosmic dust collectors will undoubtedly include extremely low density target materials such as silica aerogel as the decelerating and arresting medium. This material has been found to be clean from the point of view of inorganic elements and is thus acceptable for the purpose of harvesting grains to be studied by, for example PIXE, INAA, or SXRF. However, the process used in making aerogel leaves substantial carbon and hydrogen containing residues which would negate their suitability for collection and subsequent investigation of the very important CHON particles. Attempts to precondition aerogel by solvent extraction or heating at 500 C and 750 C in air for 24 hours or under a vacuum of 2(7)(exp -7) torr at 260 C were largely ineffective except that pyrolysis did reduce volatile species. In this investigation we have examined the use of supercritical fluids for the purpose of extracting organic residues. The logic of the new approach is that beyond the supercritical point a substance has the solvating properties of a liquid but the viscosity characteristics of a gas. For example carbon dioxide becomes supercritical at a pressure of 73 atmospheres and a temperature of 31 C; in consequence it can transform to a very powerful and ultraclean solvent. It can dissolve organic matter from low molecular weight up to molecules containing 90 carbon atoms. On release of pressure the fluid reverts to a gas which can easily be pumped away and removed from the substrate being extracted.

Huang, Hui-Ping↗

Multielement analysis of interplanetary dust particles using TOF-SIMS

Sections of three stratospheric particles (U2015G1, W7029*A27, and L2005P9) were analyzed with TOF-SIMS (Time Of Flight-Secondary Ion Mass Spectrometry) continuing our efforts to investigate the element distribution in interplanetary dust particles (IDP's) with high lateral resolution (approximately 0.2 micron), to examine possible atmospheric contamination effects, and to further explore the abilities of this technique for element analysis of small samples. The samples, previously investigated with SXRF (synchrotron X-ray fluorescence analysis), are highly enriched in Br (Br/Fe: 59 x CI, 9.2 x CI, and 116 x CI, respectively). U2015G1 is the IDP with the by far highest Zn/Fe-ratio (81 x CI) ever reported in chondritic particles.

Stephan, T.↗

The anatomy of a cluster IDP. Part 1: Carbon abundance, bulk chemistry, and mineralogy of fragments from L2008#5

The objective of this study was to determine whether or not cluster particles are sufficiently homogeneous to enable observations from one fragment of the cluster to be extrapolated to the entire cluster. We report on the results of a consortium study of the fragments of a large cluster particle. Multiple fragments from one large cluster were distributed to several research groups and were subjected to a variety of mineralogical and chemical analyses including: SEM, TEM, ion probe, SXRF, noble gas measurements, and microprobe laser mass spectrometry of individual fragments.

Thomas, K. L.↗

Collection requirements for trace-element analyses of extraterrestrial samples

Trace-element abundances have proven important in understanding the evolution of and interrelationships between different meteorites. Preliminary investigations of the trace-element contents of interplanetary dust particles indicate that trace-element abundances will prove equally important in distinguishing between micrometeorites of different types, comparing the interplanetary dust to the meteorites, and assessing the degree of thermal alteration experienced either on the parent body or during the collection process. Sample collection, delivery, and curation must be accomplished in a manner to avoid contamination with even trace amounts of the elements to be analyzed. The present SXRF sensitivity for micrometeorite analysis is of order 1 femtogram, but anticipated improvements in sensitivity will require sample contamination substantially below this level. Sample collection and handling equipment should be constructed from materials selected for ultrahigh purity, and serious consideration should be given in selecting the particular set of elements from which the collection apparatus is composed so as not to compromise useful information.

Flynn, George J.↗

Characterization of Three Carbon- and Nitrogen-Rich Particles from Comet 81P/WILD

Comets may sample the early solar system s complement of volatile-forming elements - including C and N - more fully and reliably than do the terrestrial planets or asteroids. Until recently, all elemental analyses of unambiguously cometary material were carried out remotely. The return of the Stardust mission makes it possible to analyze documented material from P81/Wild 2 in the laboratory Wild 2 particles fragmented when they stopped in the aerogel collectors. We have studied three fragments thought to be rich in C and N by using several techniques: FTIR to characterize organic matter; synchrotron-induced x-ray fluorescence (SXRF) to determine Fe and certain element/Fe ratios; SEM to image sample morphology and to detect semiquantitatively Mg, Al, Si, Ca, and Fe; and nuclear reaction analysis (NRA) to measure C, N, O, and Si.

Gallien, J.-P.↗

Stardust Interstellar Preliminary Examination (ISPE)

In January 2006 the Stardust sample return capsule returned to Earth bearing the first solid samples from a primitive solar system body, C omet 81P/Wild2, and a collector dedicated to the capture and return o f contemporary interstellar dust. Both collectors were approximately 0.1m(exp 2) in area and were composed of aerogel tiles (85% of the co llecting area) and aluminum foils. The Stardust Interstellar Dust Col lector (SIDC) was exposed to the interstellar dust stream for a total exposure factor of 20 m(exp 2-) day during two periods before the co metary encounter. The Stardust Interstellar Preliminary Examination ( ISPE) is a three-year effort to characterize the collection using no ndestructive techniques. The ISPE consists of six interdependent proj ects: (1) Candidate identification through automated digital microsco py and a massively distributed, calibrated search (2) Candidate extr action and photodocumentation (3) Characterization of candidates thro ugh synchrotronbased FourierTranform Infrared Spectroscopy (FTIR), S canning XRay Fluoresence Microscopy (SXRF), and Scanning Transmission Xray Microscopy (STXM) (4) Search for and analysis of craters in f oils through FESEM scanning, Auger Spectroscopy and synchrotronbased Photoemission Electron Microscopy (PEEM) (5) Modeling of interstell ar dust transport in the solar system (6) Laboratory simulations of h ypervelocity dust impacts into the collecting media

Westphal, A. J.↗

Mineralogy of Interplanetary Dust Particles from the Comet Giacobini-Zinner Dust Stream Collections

The Draconoid meteor shower, originating from comet 21P/Giacobini-Zinner, is a low-velocity Earth-crossing dust stream that had a peak anticipated flux on Oct. 8, 2012. In response to this prediction, NASA performed dedicated stratospheric dust collections to target interplanetary dust particles (IDPs) from this comet stream on Oct 15-17, 2012 [3]. Twelve dust particles from this targeted collection were allocated to our coordinated analysis team for studies of noble gas (Univ. Minnesota, Minnesota State Univ.), SXRF and Fe-XANES (SSL Berkeley) and mineralogy/isotopes (JSC). Here we report a mineralogical study of 3 IDPs from the Draconoid collection..

Nakamura-Messenger, K.↗