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A micro-Raman and infrared study of several Hayabusa category 3 (organic) particles
© Kitajima et al.; licensee Springer. 2015
Received: 1 May 2014
Accepted: 6 January 2015
Published: 11 February 2015
Three category 3 (organic) particles (RB-QD04-0001, RB-QD04-0047-02, and RA-QD02-0120) and so-called ‘white object’ found in the sample container have been examined by micro-Raman and infrared (IR) spectroscopy. In addition, several artificial substances that could occur as possible contaminants and chondritic insoluble organic matter (IOM) prepared from the Murchison CM2 chondrite were analyzed. The Raman spectra of the particles show broad G-band and weak D-band. The G-band parameters plot in the disordered region and close to the artifact produced from a Viton glove after laser exposure rather than chondritic IOM. The particles were therefore originally at low maturity level, suggesting that they have not experienced strong heating and are therefore not related to the LL4-6 parent body. The IR spectra are not similar to that of chondritic IOM. Furthermore, the particles cannot be identified as some artificial carbonaceous substances, including the white object, which are the possible contaminants, examined in this investigation. Although it cannot be determined exactly whether the three category 3 particles are extraterrestrial, the limited IR and Raman results in this investigation strongly suggest their terrestrial origin. Although they could not be directly related to the artificial contaminants examined in this investigation, they may yet be reaction products from similar substances that flew on the mission. In particular, RB-QD04-0047-02 shows several infrared spectral absorption bands in common with the ‘white object.’ This may relate to the degradation of a polyimide/polyamide resin.
The Hayabusa space craft returned to the Earth on 13 June 2010 from the Muses-C region on the asteroid Itokawa with more than 1,500 tiny particles (e.g., Nakamura et al. 2011). Subsequently, more than 450 particles have been picked up from the sample catcher (Uesugi et al. 2014). The recovered particles have been classified into four categories (Yada et al. 2014). Categories 1 and 2 are siliceous particles, and category 3 particles are carbonaceous. Category 4 particles are artificial materials such as aluminum flakes (Yada et al. 2014), and the so-called ‘white object’ found in the sample container (http://hayabusaao.isas.jaxa.jp/catalog/contaminations.pdf) may be also included in this category.
Category 1 particles are composed only of transparent minerals, whereas category 2 particles consist of not only transparent particles but also opaque minerals (Yada et al. 2014). Particles belonging to categories 1 and 2 have been confirmed as Itokawa regolith (e.g., Ebihara et al. 2011; Nagao et al. 2011; Nakamura et al. 2011; Noguchi et al. 2011; Tsuchiyama et al. 2011; Yurimoto et al. 2011).
The asteroid Itokawa belongs to S-type and its surface has been considered to have an olivine-rich mineral assemblage similar to that of LL5 chondrite (Abe et al. 2006; Hiroi et al. 2006). The returned stony samples confirm that Itokawa is indeed an ordinary chondrite parent body of grade LL4-6 (Nakamura et al. 2011). Although average concentrations of 0.04% to 0.19% carbon in matrices of LL4-6 chondrites have been reported (Makjanic et al. 1993), carbonaceous matter in such chondrites is expected to be depleted and thermally altered. However, Itokawa is a rubble-pile object; therefore, primitive carbon-rich fragments could also be present, besides more mature carbonaceous matter. Several stony particles were examined in search of such organic materials; however, any amino acids (Naraoka et al. 2012) or insoluble organic matter (IOM) of extraterrestrial origin have not yet been found (Kitajima et al. 2011) on the surface of these particles.
Besides the silicate particles, several carbon-rich particles classified into category 3 have been found in the sample catcher (e.g., Yada et al. 2014; Uesugi et al. 2014). The particles are mainly composed of carbon and often contain oxygen, nitrogen, and sulfur (Yada et al. 2014). It has not yet been clarified whether these particles are extraterrestrial in origin. In this investigation, as a part of the sequential analysis of category 3 particles, we examined three category 3 particles (RB-QD04-0001, RB-QD04-0047-02, and RA-QD02-0120) by micro-Raman and Fourier transform infrared (FTIR) spectroscopies, together with several artificial carbonaceous substances including the ‘white object’ found in the sample container. The artificial substances are analyzed in order to get a clue as to whether the category 3 particles are extraterrestrial or not, and our data should be coupled with the results of other kinds of analyses (NanoSIMS, time-of-flight secondary ion mass spectrometry (ToF-SIMS), and X-ray absorption near edge structure (XANES) described in a series of articles in this issue (Uesugi et al. 2014; Ito et al. 2014; Yabuta et al. 2014; Naraoka et al. 2015).
Category 3 particles
Out of 457 recovered particles, 58 have been classified into category 3 (Uesugi et al. 2014). The particles were mainly composed of C, N, and O and further classified into three subtypes, types 1 to 3, as blocky, fibrous, and faint, respectively (Uesugi et al. 2014). Three category 3 particles (RB-QD04-0001, RB-QD04-0047-02, and RA-QD02-0120) were analyzed in this study. RB-QD04-0001 belongs to faint type. It is 19 μm in size. C, N, and O are observed by FE-SEM-EDS. RB-QD04-0047-02 belongs to blocky type, 28 μm in size, and contains C and O. RA-QD02-0120 also belongs to the blocky type, 26 μm in size, and contains C and O. Further analyses by TEM/STEM (Uesugi et al. 2014), N-XANES (Yabuta et al. 2014), and H, C, and N isotopic investigation (Ito et al. 2014) revealed the presence of N in the RB-QD04-0047-02 and RA-QD02-0120 particles. A detailed description of the category 3 particles is given in Uesugi et al. (2014). Because the particles must be fixed in some manner for the NanoSIMS and ToF-MS analyses planned as parts of a sequential analysis, they were pressed onto gold plates (Uesugi et al. 2014) at the PMSCF/JAXA (The Planetary Material Sample Curation Facility of JAXA). The particles RA-QD02-0120 and RB-QD04-0047-02 were also investigated by XANES analyses (Yabuta et al. 2014). Calcium carbonate inclusions of up to 300 nm have been identified in RA-QD02-0120 by TEM/STEM (Uesugi et al. 2014) as well as C and Ca by XANES (Yabuta et al. 2014). The particle RB-QD04-0047-02 was also analyzed by ToF-SIMS (Naraoka et al. 2015); TEM/STEM observation (Uesugi et al. 2014) and ToF-SIMS analysis pointed out a wide but heterogeneous distribution of Si. One particle, RB-QD04-0001, was allocated in the initial analysis, and the intact particle had also been examined using a diamond holder previously. Although the collected spectra have not been definitive, O-H stretching at 3,239 cm−1 and several absorption bands in 1,700 to 1,277 cm−1 region have been observed. These absorption bands may be in common with RA-QD02-0008. The results of the analysis using the diamond holder will be reported in detail elsewhere. Because solvent extraction has not been investigated, whether the particles are soluble or insoluble in organic solvents has not yet been clarified.
Artificial carbonaceous substances and the ‘white object’
At least two types of extraterrestrial organic materials can be expected in the Itokawa particles. One is a thermally mature material that would have been contained in the original Itokawa parent body. The other is a rather primitive carbonaceous material that would be transported from space. Because IOM from the LL4-6 chondrites is scarce (in types 3.6 to 3.7 ordinary chondrites, most IOM has disappeared; Busemann et al. 2007), the IOM sample was prepared from the Murchison CM2 chondrite as a primitive extraterrestrial material for comparison. The preparation method is described in Oba and Naraoka (2009). The sample was pressed onto a copper plate for the measurement at Kyushu University.
One category 3 particle, RA-QD02-0120, was analyzed at PMSCF/JAXA. The other particles were analyzed at Kyushu University. The particle RB-QDO4-0001 had been crushed and scattered on the gold plate; therefore, two regions named RB1 and RB2 were analyzed. Mid-IR reflectance spectra of RA-QD02-0120 were obtained using a JASCO FTIR-6100 spectrometer with a mercury-cadmium-telluride (MCT) detector at PMSCF/JAXA. A total of 1,024 scans of spectra were accumulated with a 25 × 25 μm2 aperture. The IR spectra of the other samples were collected using a Perkin-Elmer Spectrum One spectrometer (PerkinElmer Inc., Waltham, MA, USA) with a MCT detector. The same total scans of the spectra were accumulated with the same aperture size. The reflectance spectra of the category 3 particles on gold plate and the IOM from the Murchison chondrite on the copper plate were collected. The reflectance spectra of Tufram were obtained by measuring the surface of a spare rotational cylinder of the Hayabusa sample container. The transmission spectra of the Viton rubber and the white object on diamond plate (0.2 μm thickness) were also collected. Commercial Kapton 120HR616 film was analyzed without the diamond plate. IR measurements were performed prior to the Raman analyses to avoid sample damage that would be caused by laser exposure. Raman spectra were obtained using JEOL JRS system 2000 Raman spectrometer (JEOL Ltd., Tokyo, Japan) (1,800 lines/mm grating). An excitation wavelength of 514.5 nm was used on an argon ion laser. The laser beam was focused by a microscope equipped with a × 50 or × 100 objective, leading to a spot diameter of 2 or 1 μm. Three scans of spectra of the Murchison IOM were accumulated with a 10-s exposure. A scan of spectrum of the Viton rubber with a 10-s exposure was also obtained. The laser power at the outlet of the light source was 20.3 mW, and on the sample surface was 1.0 mW. Five scans of spectra of the two category 3 particles, RB-QD04-0047-02 and RB-QD04-0001, were accumulated with a 2-s exposure. Five points were analyzed for each particle (five points for each region from RB-QD04-0001). The power on the sample surface was 0.2 mW, which was reduced more than usual because the particles might be sensitive to heating. Following analysis, we observed that no hole was burnt through the sample surface and the spectral features did not transform during accumulation; therefore, we consider that laser damage is negligible (five scans with a 2-s exposure at the power of 0.2 mW on the sample surface did not show laser-induced alteration of the Viton rubber). Raman spectrum of RA-QD02-0120 was obtained with a JASCO NRS-5100 Raman spectrometer (JASCO Corporation, Tokyo, Japan) (1,800 lines/mm grating) at PMSCF/JAXA. An excitation wavelength of 532.18 nm was used on an argon ion laser. The laser beam was focused by a microscope equipped with a × 50 objective. The power on the sample surface was lower than 0.1 mW. Ten scans of the spectra with 30 s exposure were accumulated. All measurements were performed in the atmosphere. The curve fitting for the Raman spectra was performed using the pseudo-Voigt function after subtraction of the linear baseline.
Results and discussion
The category 3 particles
The Raman spectrum indicates the structural order of carbonaceous matter. Ideal monocrystalline graphite shows only the so-called G-band at 1,581 cm−1. Depending on the level of disorder, the G-band shifts to higher wavenumbers and can be observed at around 1,600 cm−1 (e.g., Sandford et al. 2006; Busemann et al. 2007; Quirico et al. 2009). The so-called D-band at around 1,350 cm−1 is not present in the perfectly stacked graphite and it is induced by structural defects. Its size reflects increasing disorder (Busemann et al. 2007; Quirico et al. 2009).
Viton glove (CC2#8)
The IR spectra of the category 3 particles differ from that of Viton glove in the absence of C-F stretching at 1,151 cm−1. F-XANES analysis of RB-QD04-0047-02 shows the absence of fluorine (Yabuta et al. 2014), being consistent with this IR observation. Therefore, the particles are, at least, not ‘fresh’ fragments of the Viton rubber itself.
Figure 8c shows the IR spectrum of Tufram that is used for the surface coating of the rotational cylinder of the Hayabusa sample container. The strong absorption band at 1,259 cm−1 of C-F stretching of PTFE shown by this material is also not observed in the category 3 particles (the absorption band at 1,252 cm−1 shown by RB-QD04-0047-02 cannot be related to PTFE because of the absence of fluorine indicated by F-XANES).
Comparison between category 3 particles and artificial substances
Raman G-band diagram and thermal maturity
The category 3 particles as thermally unaltered materials
H, C, and N isotopic compositions can be sensitive indicators for determining the provenance of primitive extraterrestrial carbonaceous matter. The three category 3 particles however have been reported to show terrestrial H, C, and N isotopic compositions within errors, and micrometer-sized hot spots with anomalous H, C, and N compositions have not been found (Ito et al. 2014). However, these observations are not enough to determine whether the particles are terrestrial contaminants or extraterrestrial matter, because isotopically normal carbonaceous material has been also reported in IDPs and Antarctic micrometeorites (Messenger 2000; Yabuta et al. 2013). When isotopic anomalies are not found, a simple and conclusive method to determine whether a carbonaceous substance is extraterrestrial has not yet been established, excluding the materials that would show enantiomer excess such as amino acids and monosaccharides. If it cannot be identified as a man-made substance, it should be confirmed that the elemental composition, structure, and provenance are consistent with extraterrestrial origin.
The IR spectra of the two category 3 particles, RB-QD04-0047-02 and RB-QD04-0001, seem not to have the characteristics of the unheated chondritic IOM. Further, the spectral features of the two particles are not similar to known extraterrestrial carbonaceous matter heated or unheated. In addition, no IR spectra of artificial carbonaceous substances including the white object show exactly the same spectral features as the category 3 particles. Although it is difficult to determine definitively whether the particles are extraterrestrial in origin based on these limited results, their terrestrial origin(s) is/are suggested. They may be some reaction products from such artificial substances; however, the lack of C-F stretching indicates that all the category 3 particles are not ‘fresh’ contaminants from Viton, PTFE, and Tufram derived from the curation facilities.
RA-QD02-0120 does not seem to originate from a thermally altered parent body; however, IR and Raman data are not clear enough to clarify further its origin. The aliphatic C-H stretching of RA-QD02-0120, taking into account the presence of calcium carbonate (Uesugi et al. 2014; Yabuta et al. 2014), suggests various origins of the category 3 particles, although this particle belongs to the same subtype (blocky) as RB-QD04-0047-02. However, polyimide/polyamide resin is a major candidate for the source material of the particles. If several category 3 particles could be consumed, chemical degradation and analysis of the products using HPLC/HRMS could be of great help. The behavior of the resin during sample return should be clarified in order to determine the origin(s) of the category 3 particles.
The Raman spectra of the category 3 particles showed both G- and D-bands. In the G-band diagram, the parameters plot in the disordered region, suggesting that the three category 3 particles, RB-QD04-0047-02, RB-QD04-0001, and RA-QD02-0120, are not thermally altered substances. The particles are not likely to have originated from an LL4-6 parent asteroid. The particles plot close to the laser-induced artifact of Viton rubber rather than the Murchison IOM. The Raman results of the particles are not similar to known extraterrestrial carbonaceous matter heated or unheated. The IR spectral features of the RB-QD04-0047-02 and RB-QD04-0001 are also not similar to the Murchison IOM. The IR result of RA-QD02-0120 is not sufficiently clear. Although it cannot be determined whether they are extraterrestrial or not by these limited results, their terrestrial origin is suggested.
They were not identified as being the same as the artificial contaminants examined in this investigation. The lack of C-F stretching indicates the category 3 particles are not ‘fresh’ contaminants of Viton, PTFE, and Tufram at the curation facilities. They may be reaction products from artificial substances exposed to radiation during the sample return. In particular, RB-QD04-0047-2 may be a mixture of polyimide/polyamide resin as is the white object. It has several IR spectral absorption bands in common with the white object. It may relate to a degradation of polyimide/polyamide resin. RB-QD04-0001 may also relate to the resin. Although RA-QD02-0120 suggests a different origin and the category 3 particles may have various origins, it is necessary to clarify the behavior of polyimide/polyamide resin during sample return in order to determine the origin(s) of the category 3 particles.
We appreciate the two anonymous reviewers for their comments to improve the manuscript. We also thank to official editor Trever Ireland for helpful comments and editorial handling.
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