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Sobron Et Al., 2012 This article appeared in a journal published by Elsevier. The attached copy is furnished to the author for internal non-commercial research and education use, including for instruction at the authors institution and sharing with colleagues. Other uses, including reproduction and distribution, or selling or licensing copies, or posting to personal, institutional or third party websites are prohibited. In most cases authors are permitted to post their version of the article (e.g. in Word or Tex form) to their personal website or institutional repository. Authors requiring further information regarding Elsevier’s archiving and manuscript policies are encouraged to visit: http://www.elsevier.com/copyright Author's personal copy Spectrochimica Acta Part B 68 (2012) 1–16 Contents lists available at SciVerse ScienceDirect Spectrochimica Acta Part B journal homepage: www.elsevier.com/locate/sab Extraction of compositional and hydration information of sulfates from laser-induced plasma spectra recorded under Mars atmospheric conditions — Implications for ChemCam investigations on Curiosity rover Pablo Sobron a,⁎, Alian Wang a, Francisco Sobron b a Department of Earth and Planetary Sciences and McDonnell Center for the Space Sciences, Washington University, St. Louis, MO 63130, USA b Unidad Asociada UVa-CSIC a traves del Centro de Astrobiología, Parque Tecnológico de Boecillo, Parcela 203, Boecillo (Valladolid), 47151, Spain article info abstract Article history: Given the volume of spectral data required for providing accurate compositional information and thereby in- Received 13 July 2011 sight in mineralogy and petrology from laser-induced breakdown spectroscopy (LIBS) measurements, fast Accepted 2 January 2012 data processing tools are a must. This is particularly true during the tactical operations of rover-based plan- Available online 21 January 2012 etary exploration missions such as the Mars Science Laboratory rover, Curiosity, which will carry a remote LIBS spectrometer in its science payload. We have developed: an automated fast pre-processing sequence Keywords: of algorithms for converting a series of LIBS spectra (typically 125) recorded from a single target into a reli- LIBS Martian sulfates able SNR-enhanced spectrum; a dedicated routine to quantify its spectral features; and a set of calibration Composition curves using standard hydrous and multi-cation sulfates. These calibration curves allow deriving the elemen- Hydration state tal compositions and the degrees of hydration of various hydrous sulfates, one of the two major types of sec- Calibration curve ondary minerals found on Mars. Our quantitative tools are built upon calibration-curve modeling, through the correlation of the elemental concentrations and the peak areas of the atomic emission lines observed in the LIBS spectra of standard samples. At present, we can derive the elemental concentrations of K, Na, Ca, Mg, Fe, Al, S, O, and H in sulfates, as well as the hydration degrees of Ca- and Mg-sulfates, from LIBS spec- tra obtained in both Earth atmosphere and Mars atmospheric conditions in a Planetary Environment and Analysis Chamber (PEACh). In addition, structural information can be potentially obtained for various Fe- sulfates. © 2012 Elsevier B.V. All rights reserved. 1. Introduction detect and to quantify the concentration of major, minor, and often trace elements present in a sampling target. The accuracy and preci- Laser-induced breakdown spectroscopy (LIBS) is recognized as a sion of the quantification of elemental concentrations based on LIBS powerful tool for detailed geochemical investigations of rocks and measurements are influenced mainly by two factors: the matrix ef- regolith and for exploratory survey in future landed missions on plan- fects within a specific sample and the fluctuations in experimental etary bodies including Mars [1], the Moon [2], and Venus [3,4].A conditions. A good explanation of the matrix effects in LIBS was stand-off LIBS spectrometer is part of the ChemCam instrument [5], given in Cremers and Radziemski [6]. They grouped the matrix effect included in the scientific payload of NASA's Mars Science Laboratory into two kinds: physical and chemical matrix effects. On one hand, (MSL) rover (named Curiosity), that was launched in late 2011. physical matrix effects, related to the physical properties of the target ChemCam will determine the chemical composition of rocks and reg- (e.g., grain size, surface roughness, absorptivity and thermal conduc- olith on Mars at distances ranging from 1 to 7 m. tivity). Physical matrix effects complicate quantitative analysis with The LIBS technique is particularly well suited for planetary explo- LIBS by causing uncontrolled random fluctuations in the emission ration, as it is sensitive to all rock-forming elements, as well as H, C, N, from the plasma. On the other hand, chemical matrix effects, related O, S, P, Fe, and Cl, relevant to the search for habitable environments to the elemental and molecular compositions of the sample. They and for traces of past and present signs of life on Mars. In LIBS, the can result in higher emission from easily ionized elements existing wavelength and the intensity of atomic emission lines are used to in the matrix, i.e., the same concentration of an element in different matrices will result in emission lines with different intensities, thus affecting the accuracy of compositional quantification using LIBS ⁎ Corresponding author at: Space Science & Technology, Canadian Space Agency, 6767 data. As for the fluctuations in experimental conditions, they include Rte. de l'Aéroport, St. Hubert, QC, Canada J3Y 8Y9. Tel.: +1 450 926 5847; fax: +1 450 926 4766. pulse-to-pulse variations in the properties of laser beam (pulse fre- E-mail addresses: [email protected], [email protected] (P. Sobron). quency, pulse width, and energy density), variations in laser-to- 0584-8547/$ – see front matter © 2012 Elsevier B.V. All rights reserved. doi:10.1016/j.sab.2012.01.002 Author's personal copy 2 P. Sobron et al. / Spectrochimica Acta Part B 68 (2012) 1–16 sample optical path (e.g., accidental scatters), and variations in and electron density of the plasma created by the laser pulse. In CF- sample-to-collection optics optical path (including atmospheric ef- LIBS, local thermodynamic equilibrium (LTE) is assumed. Note that fects). The latter two can be considered physical matrix effects as LTE and other conditions relevant to CF-LIBS have been verified [16]. well, since they are mainly due to random effects in the laser ablation In this paper we describe a methodology for general automated phase and contribute strongly to the standard deviation of LIBS mea- pre-processing and quantitative analysis of LIBS spectral data and re- surement by modifying the collection angles. port its step-by-step application to construct a set of calibration All the factors mentioned above compromise the reproducibility curves for common elements in sulfate matrix under Mars and of LIBS measurements and the accuracy of quantitative calculations Earth atmospheric conditions. We also show the application of the based on LIBS data. To compensate for matrix effects and variations calibration curves to characterize two natural sulfate-bearing sam- in experimental conditions, normalization procedures are commonly ples. At the time this manuscript was prepared, matrix-specific cali- employed [1,6,7]. In most normalization approaches, the intensity of a bration curves for additional matrices relevant to Mars (basalts, measured peak is normalized to that of another peak in the same phyllosilicates, carbonates, etc.) are under construction. spectrum that is known to reflect spectral changes due to matrix ef- fects [1,6]. However, in applications where such internal standard does not exist (e.g., most mineralogical analyses of geological sam- 2. Experimental ples, such as ChemCam measurements on Mars), normalization by the total emission intensity of the spectrum is preferred (e.g., [7]). 2.1. Sulfate standard samples for the construction of calibration curves In the preceding paragraphs we have emphasized those factors that affect quantitative analyses of targets. By quantitative analyses Sulfates were selected for the development of this first set of cali- we mean a series of mathematical operations performed on a LIBS bration curves because they are one of the two major types of second- spectrum that aim to reconstruct the stoichiometry of a target inter- ary minerals found on Mars that may provide potentially habitable rogated by the laser, i.e., to determine the elemental abundances in environments due to their association with ancient aqueous environ- a sample. Most common quantitative analysis methods use calibra- ments in which life might have thrived. In this work we used pure hy- tion procedures to generate calibration curves for one or several ele- drous sulfates with multiple cations synthesized in previous studies ments from the spectra of standard samples in a specific matrix, each by the authors [17,18], and several commercial-grade sulfates. These sample containing precisely known concentrations of the elements of sulfates are used as standards to establish the calibration curves interest [8]. Different calibration curves are often constructed for dif- based on their LIBS spectra obtained under Mars atmospheric condi- ferent matrices. The concentrations of the elements in unknown sam- tions. All of the samples, including their provenance and the atomic ples are determined from the calibration curves by a quantitative fractions of the elements relevant for this work calculated from X- measure of certain spectral features in their spectra. An alternative ray fluorescence measurements (described below), are listed in approach to the quantitative analysis of LIBS spectra is multivariate Table 1. A manual pellet press was used to apply ~4 tons of pressure analysis (MVA), i.e., the simultaneous analysis of more than one sta- to the powdered samples, which were placed in compressible alumi- tistical variable. MVA is widely used and seems to be preferred for num cups (Chemplex Industries, Inc. PelletCups) to form solid bri- the study of materials relevant to Mars exploration [9,10].
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