Microlite Orientation in Obsidian Flow Measured by Synchrotron X-Ray Diffraction
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Contributions to Mineralogy and Petrology _#####################_ https://doi.org/10.1007/s00410-018-1479-9 Revised Proof ORIGINAL PAPER Microlite orientation in obsidian flow measured by synchrotron X-ray diffraction Michael Manga1 · Marco Voltolini2 · Hans‑Rudolf Wenk1 Received: 16 April 2018 / Accepted: 31 May 2018 © Springer-Verlag GmbH Germany, part of Springer Nature 2018 Abstract Clinopyroxene and plagioclase (andesine) microlites in an obsidian flow from Glass Mountain (NE California, USA) display strong alignment. Synchrotron X-ray diffraction, coupled with Rietveld analysis, was used to quantify crystallographic- preferred orientation (CPO). Clinopyroxene, with a rod-shaped morphology, shows a strong alignment of [001] in the flow direction and (010) aligned parallel to the inferred flow plane. Andesine, with a platy morphology, displays an alignment of (010) platelets in the flow plane. Some pole densities exceed 90 multiples of random distribution. Applying a model of rigid ellipsoidal inclusions in a viscous matrix, the local pure shear strains are between 2 and 3. Keywords Obsidian · Microlite alignment · Texture analysis · Crystal-preferred orientation, Strain estimates Introduction (e.g., Manga 1998; Castro et al. 2004). Because microlites are small, however, it is not usually possible to determine Obsidian in natural lava flows preserves a number of tex- crystallographic orientation, and microlites with diameters tural features that record its eruption and emplacement (e.g., smaller than about 1 µm cannot be characterized. Here, we Smith 2002). Structural features range from folds and layer- use synchrotron X-ray diffraction and scanning electron ing at centimeter-to-decameter scales (Fink 1983; Manley microscopy to investigate two rhyolitic obsidian samples and Fink 1987; Castro and Cashman 1999), to deformed from the Glass Mountain lava flow, Medicine Lake Volcano, bubbles at the micrometer-to-millimeter scale (e.g., Rust Northern California. et al. 2003; Gardner et al. 2017) and aligned elongated Synchrotron hard X-ray diffraction proved to be a very micrometer-sized crystallites at the smallest scales (Manga useful method for texture analysis in a broad range of differ- 1998; Castro et al. 2002). Together, these textures provide ent materials from metals (e.g., Wu et al. 2010) to complex information about flow, fragmentation, and solidification clays (e.g., Wenk et al. 2010), slates (e.g., Haerinck et al. processes. 2015), and serpentinite (e.g., Soda and Wenk 2014). This Microlites are oriented by flow, and their orientation dis- is a first application of the method to volcanic rocks. Con- tribution thus offers an opportunity to determine the type of trary to optical microscopy referred to above that describes flow and strain experienced by the melt prior to quenching the shape-preferred orientation (SPO) of particles, X-ray (e.g., Castro et al. 2002; Befus et al. 2014, 2015). Quanti- texture analysis provides a quantitative description of the tative information, including the relationship between size crystallographic orientation distribution of clinopyroxene and orientation, can be obtained with optical microscopy and plagioclase, averaging over crystallite volumes, not over crystallite numbers. The analysis is by no means trivial in the case of obsidian, since crystallites contribute less than Communicated by Timothy L. Grove. 2% of the volume and diffraction from those crystals is weak * Hans-Rudolf Wenk compared to scattering from the amorphous glass. Never- [email protected] theless, results for SPO and CPO are comparable and can be used to estimate local strain patterns based on Jeffery’s 1 Department of Earth and Planetary Science, University (1922) solution for the motion of rigid ellipsoidal inclusions of California, Berkeley, CA 94720, USA in a viscous matrix. 2 Earth and Environmental Sciences Area, Lawrence Berkeley National Laboratory, Berkeley, CA 94720, USA Vol.:(0123456789)1 3 _####_ Page 2 of 12 Contributions to Mineralogy and Petrology _#####################_ Revised Proof Experimental Sample 2 was also analyzed with a JEOL SEM at the Engineering Department of the University of Trento, Italy, Samples to identify the phases and determine their morphology. Back-scattered images, again parallel and perpendicular The two samples investigated are obsid- to the flow direction, are shown in Fig. 3. Pyroxenes are ian fragments from Glass Mountain, CA, USA easily recognized, with high contrast. They are prismatic (41°36′15.5″N/121°28′34.5″W). This ~ 1 km3 compo- needles with a pseudohexagonal cross section, roughly sitionally zoned flow erupted about 1070 AD and is the 2–10 µm long and 0.1–2 µm in diameter. Contrast for pla- youngest eruption at the Medicine Lake shield volcano gioclase is weak because of a similar chemical compo- (Grove et al. 1997, Donnelly-Nolan et al. 2016). Optical sition as the glass matrix. Some crystals are marked in microscopy reveals a layered structure with layers 2–5 mm Fig. 3. They are larger than pyroxenes and have a platelet in thickness (Fig. 1a). Some layers are more uniform than morphology (see also Fig. 2). They range in size from 2 others. At higher magnification, a strong alignment of to 25 µm long to 2–5 µm wide. The chemical composi- needle-shaped microlites is apparent (Fig. 1b). Locally, tions of the phases were analyzed with an EDAX EDS there is distorted flow around larger inclusions of magnet- system (Fig. 4; Table 1). The pyroxene is identified as fer- ite (Fig. 1c) and fragments of plagioclase (Fig. 1d). rous intermediate augite/pigeonite (Ca0.18, Mg0.43, Fe0.36, In this study, we focus on homogeneous layers in two Na0.03) SiO3, plagioclase as calcic andesine (Ca0.40 Na0.52 samples. In sample 1, microlites are almost exclusively K0.08)(Si0.72, Al0.28)O8, and glass as high in SiO2 (> 70%) clinopyroxene (Fig. 1b). Sample 2 is a mixture of pla- with significant aluminum, potassium, and sodium. gioclase and clinopyroxene microlites. Views of sample 2 with plane polarizers (Fig. 2a, c) and crossed polarizers Hard X‑ray synchrotron diffraction (Fig. 2b, d), both parallel to the flow direction (Fig. 2a, b) and perpendicular to the flow direction (Fig. 2c, d), show Samples for the X-ray diffraction experiment were ~ 0.7 mm- the morphology and the strong alignment of microlites. thick slabs with the flow plane perpendicular to the slab Clinopyroxenes are needles aligned in the flow direction surface. The diffraction measurements were carried out at and plagioclase microlites are platelets aligned in the flow beamline 11-ID-C at the Advanced Photon Source (APS) of plane. Plagioclase platelets are typically larger in size than Argonne National Laboratory. Experiments were performed clinopyroxene needles which is most obvious with crossed in transmission geometry. A beam of X-rays (λ = 0.10738 Å), polarizers. 0.5 mm in diameter, irradiates the sample, and diffraction patterns were recorded by a Mar345 image plate detector Fig. 1 Optical micrographs of obsidian in sample O1. Plane polarized light. a Structure with compositional layering (Os2a), b detail of layering with microlites, c microlites around an inclusion of magnetite, and d inclusion of plagioclase. In c, the curves show streamlines for pure shear around a spherical and rigid inclusion 1 3 Contributions to Mineralogy and Petrology _#####################_ Page 3 of 12 _####_ Revised Proof Fig. 2 Optical micrographs of obsidian in sample O2, a, b parallel to the flow direction and c, d perpendicular to the flow direction;a, c are plane polarized light and b, d crossed polarizers. Microlites are andes- ine (And) and clinopyroxene needles (lines in a and dots in c). In the upper right corner of a and c, an enlarged segment is displayed (3450 × 3450 pixels) placed about 2 m behind the sample. First, instrumental parameters such as sample detector Exposure time was 900 s. High energy maximizes sample distance, detector orientation, and Caglioti parameters defin- penetration. The beam size was chosen to give a sufficiently ing the diffraction resolution were refined from diffraction 3 large sample volume (~ 0.2 mm ) to be representative of a data collected for a CeO 2 standard. These instrument param- single flow layer. The diffraction images display Debye rings eters were then applied to each of the four obsidian sample that have intensity variations as a function of the azimuth data sets. because of preferred orientation of crystallites (Fig. 5). A The Rietveld refinement requires as input the crystallo- dark broad ring is due to scattering from glass and sharp graphic characterization of the composing phases. For clino- rings are scattering from crystallites. pyroxene, the C2/c structure was used (Clark et al. 1969, # The sample slab was mounted on a goniometer and was 1000035). For the texture analysis of monoclinic crystals in rotated around a horizontal axis perpendicular to the flow MAUD, the first setting (z monoclinic axis) has to be applied plane and the incident X-ray beam. The sample was tilted in (Matthies and Wenk 2009), but results are shown in the more 15° increments to seven positions (− 45°, − 30°, − 15°, 0°, conventional second setting (y monoclinic axis). For plagio- 15°, 30°, and 45°) to obtain a good coverage of orientation clase andesine, I 1 was used which had to be converted to P 1 space for texture analysis. This results in seven diffraction (Fitzgerald et al. 1986, #9001030). The glass phase, giving images for each data set. The flow layers are perpendicular to rise to the diffuse diffraction peaks at Q ~ 1.6 and 4.3 Å−1 the tilt axis to avoid overlapping of layers at high tilt angles. (Q = 2π/d), is more difficult to describe. For some refine- For both samples, diffraction images were recorded for two ments, a nanocrystalline form of tetragonal α (low) cristo- layers (O11, O12, O22, and O25). balite (Hosemann et al. 1991, spacegroup P4 1212) was used, which was first applied to silica glass by Le Bail (1995) and Rietveld analysis later by Lutterotti et al.