Terrestrial analogs to Martian geologic conditions are being employed with data gathered during the numerous Martian rover and satellite expeditions that have occurred since the 1960s, to characterize Mars' physiological and chemical characteristics. These materials are now being used to examine a broad selection of topics, ranging from general geochemistry to the potential for human exploration of Mars.
Moreover, in the realm of material analysis, X-ray diffraction (XRD) and X-ray fluorescence (XRF) are understood to be gold standard methods. These two synergistic approaches equip the geologic domain, which ranges from research to mining, with diverse uses and applications. Contemporary research methodologies necessitate quick and precise instruments with minimal downtime, and these refinements permit core laboratories to make data acquisition and investigation more efficient.
The Thermo Scientific™ ARL™ EQUINOX 100 X-ray diffractometer (Figure 1) utilizes a bespoke Cu (50 W) or Co (15 W) micro-focus tube supported by mirror optics. The minimal wattage required by the unit permits it to be totally portable, as it does not require an external water chiller. This portability also enables inter-laboratory transportation, and negates the requirement for specific infrastructure.
Figure 1. ARL EQUINOX 100 X-ray diffractometer
The ARL EQUINOX 100 instrument offers extremely rapid data acquisition rates in comparison to competing diffractometers, as a result of its distinctive curved position sensitive detector (CPS). This calculates, in real time, all diffraction peaks synchronously, and is consequently of great utility when it comes to both reflection and transmission calculations.
The Thermo Scientific™ ARL™ QUANT’X Energy Dispersive X-ray fluorescence (EDXRF) spectrometer (Figure 2) undertakes primary filtered radiation for sample excitation, which in turn causes fluorescence of constituent elements. The ARL QUANT’X is supported by a series of eight filters, as well as unfiltered tube excitation, which is uniquely calibrated to maximize the peak-to-background ratio for elements from Na to U.
Figure 2. ARL QUANT'X EDXRF spectrometer
The instrument therefore provides versatile research-grade apparatus, that can be effortlessly modified to every application or range of elements. Utilizing a synthesis of voltage and filter (kV), which is known as the “excitation condition”, results in a unique spectrum that represents the sample.
A multi-element assessment ordinarily executes a number of excitation conditions, offering optimal excitation efficiency for a suite of elements. In EDXRF terminology, the total set of conditions constitutes the foundation of the analytical “method” for a specific sample matrix.
A sample of basalt gathered from craters located at the Moon National Monument, Idaho, USA was examined by granulating the bulk material and inserting it in a reflection sample holder. The sample, which revolved during the analysis to minimize the effects of preferred orientation, was interpreted from 0-115° 2θ under Co Kα (1.78897 Å) radiation for 30 minutes.
Raw data examination was undertaken with I_MAD. Data processing, comprising whole pattern fitting Rietveld refinement (WPF), was carried out with the use of MDI JADE 2010 furnished with the Crystallographic Open Database (COD) and AMCSD.
The same sample was scrutinized using the UniQuant standardless fundamental parameters (FP) software package. The spectrometer engaged a 50 W Rh source, which operates at voltages up to 50 kV, and is fitted with an 8 mm beam collimator. Data is gathered using a digital pulse processor on an electronically cooled SDD with 140 eV resolution and 30 mm2 x 0.45 mm active volume.
The XRF data exhibited in Table 1 implies a high P basalt principally composed of plagioclase and potassic feldspars. Alongside a reasonably low silica content, SiO2 = 43.25%, the sample is enhanced in both Fe, Fe2O3 = 19.30%, and P, P2O5 = 2.21%, more or less 2x and 10x terrestrial normal respectively (Adcock et al., 2018). The XRD raw data (Figure 3) was examined with the use of MDI JADE 2010. The data set was subjected to a WPF Rietveld refinement to attain a quantitative phase analysis (QPA) of the sample.
Table 1. XRF results
Figure 3. 30 minute raw dataset
The terminal refinement (Figure 4) had an Rwp = 6.21, with GooF = 1.25, and demonstrated the following phases: plagioclase feldspars (anorthite, albite), k-spars (orthoclase, microcline and sanidine), hematite, augite, apatite, pyroxene, and olivine (forsterite). Table 2 exhibits the phase assemblage results for the whole range of scans.
Table 2. XRD phase assemblage
Figure 4. Refined data from 4-114° 2θ using MDI JADE 2010
The trend of the phases corresponds more than adequately with the results deriving from the XRF. Plagioclase feldspars comprise 40.9% of the sample, while potassic feldspars account for a further 17.1%. The rest of the sample is constituted by hematite = 21.9%, pyroxenes = 10.7% and olivine = 1.4%.
The resolution and speed of the ARL EQUINOX 100 diffractometer supports its capacity to comprehensively analyze geologic materials, ranging from qualitative phase assemblages to full QPA. A 30 minute calculation period was selected to optimize minor phase intensities. Moreover, when supplemented with the ARL QUANT'X EDXRF spectrometer elemental date, a complete synergistic analysis of the alkaline basalt sample can be acquired.
Consequently, the ARL EQUINOX 100 benchtop diffractometer and ARL QUANT’X benchtop EDXRF spectrometer are a perfect synthesis of process applications and analytical instruments for geologic research.
Adcock et al, 2018. Craters of the Moon National Monument Basalts as Unshocked Compositional and Weathering Analogs for Martian Rocks and Meteorites. American Mineralogist. In Press.
The author would like to express their thanks to Red Rock Community College for supplying the sample this paper used. The data was collected as part of a broader study collaboration between Thermo Fisher Scientific and Red Rocks Community College.
This information has been sourced, reviewed and adapted from materials provided by Thermo Fisher Scientific - Elemental Analyzers.
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