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Combined Micro-XRF and EDS analysis on mineral samples

A combination of energy-dispersive X-ray spectrometry (EDS) on scanning electron microscopes (SEM) with benchtop micro X-ray fluorescence spectrometry (μXRF) enhances data generation for Earth and Planetary Science samples. In our example of a mineral thick section analyses of this type can be used to determine whether the exploitation of according ore deposits is commercially viable.
Samples with sizes up to 20 cm x 16 cm can be analyzed with the M4 TORNADO Micro-XRF spectrometer in a single run within ~4 hours. This could be fo instance up to 18 thick sections. The large area Micro-XRF scans can be used in locating regions of interest for additional high-resolution SEM studies. Using SEM-EDS, minerals in large areas can be classified by automated feature analysis with stage control. This analysis option combines morphological classification with chemical analysis.

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Download EDS application note #13 on Mining industries: Fast ore characterization combining benchtop Micro-XRF and automated SEM-EDS

Download application not #14 on Low energy X-ray EDS analysis of ore mineralization at high spatial resolution

Combined EDS & EBSD for Deformation Analysis

Image, Elements Ad, Garnet

The physical strength of garnets during the intense deformation of rocks is helpful in the reconstruction of geodynamic processes. The images show a garnet in a granulite facies mafic boudin that occurs enclosed in quartzite layers within amphibolite facies gneiss of the Lindås nappe, W-Norway. The high resolution EDS map emphasizes the coronitic reaction texture, which indicates that the sample passed a cooling stage and left the garnet stability field (P < 14 kbar, T < 800 °C). The inset shows the associated detailed EBSD grain average misorientation map (garnet only) revealing the strong plastic deformation affecting the garnet (misorientation legend: from 0.1° in blue to 10° in red) during subsequent deformation. High temperature plastic deformation leaves the garnet’s major element chemistry nearly unaffected, thus in chemical disequilibrium with matrix grains.

In collaboration with Dr. Dirk Spengler, Potsdam University, Germany.

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The images show a sample from a high pressure experiment. It was conducted with a multianvil press in order to investigate how deformation textures are affected by phase transformations. An EBSD phase map (raw data), an EBSD orientation map (IPF-X, only aragonite selected) and an EDS map of the same area are shown from left to right. Both EBSD datasets overlay the pattern quality map. The simultaneous EDS and EBSD measurement ensures conclusive results (calcite and aragonite can only be distinguished using EBSD).

Sample courtesy of Dr. Florian Heidelbach, Bayerisches Geoinstitut, Universität Bayreuth.

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Fast and easy Autophase for EDS

Serpentinite sample, element map, Autophase results and BSE micrograph
Element map, Autophase results and
BSE micrograph of a serpeninite sample

The images show a serpentinite sample of subcontinental mantle origin from the Ancient Tethys, now exposed in the Totalp imbricate near Davos, Switzerland mapped with a QUANTAX EDS system. The image on the upper right side is a composite element map of Mg (green), Fe (red), Ca (dark blue) and Ni (light blue) with overlaid back-scattered electron (BSE) image. The image on the lower right side shows the BSE image unmodified. The image on the left is a phase image, where areas of similar chemical composition were made visible by Autophase, a software option for the QUANTAX ESPRIT software suite. Such phase images are useful to study the distribution and modal abundances of different minerals, as well as their element composition.

Serpentinite rocks, such as the one shown here, are of special interest for the mining industry, specifically due to the presence of Ni. Nickeliferous laterite deposits can form from the weathering of serpentinites and other ultramafic material.

The element Ni is used in many industrial and consumer products, such as stainless steel and rechargeable batteries. Lateritic Ni deposits comprise 73% of the continental world Ni resources and in the future they will be the dominant source for the mining of Ni.

Sample courtesy of Emily H. Goldstein, University of Texas at Austin.

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3D chemical analysis on the µm- to cm-scale

3D chemical analysis of the Gujba meteorite
3D chemical analysis of the Gujba
meteorite obtained by µ-XRF and
SEM/EDS combined with serial
sectioning

Analyze up to 12 orders of magnitude larger samples without longer measuring times using µ-XRF and SEM/EDS with serial sectioning instead of 3D EDS focused ion beam (FIB) analysis!

The Gujba meteorite sample shown above was mapped with an M4 TORNADO µ-XRF spectrometer (36 2D-sections). Amira® Software was used for 3D reconstructions. The 3D reconstruction of the µ-XRF data (voxel size: 32x32x148 µm) shows the surfaces of Fe,Ni-metal particles in green and sulfides in red. The Ni-content of the metal particles varies from 5 wt% (dark blue) to 8 wt% (light blue). A smaller area was mapped with a QUANTAX EDS system (21 2D-sections). The 3D reconstruction of the EDS data (voxel size:1.6x1.6x4 µm) shows Fe (blue) and S (red).

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View the recording of the webinar on the analysis of the Gujba meteorite using a combination of methods

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Fast & comprehensive feature analysis

Feature Analysis Results of a Monazite Containing Sample
Feature analysis results of a monazite
containing sample, also showing a
deconvoluted REE-containing spectrum

Rare earth elements (REE) have gained increasing importance for high technology industries. The scarcity of REE on the global market makes it necessary to explore alternative resources. The laterite deposit shown above was examined using ESPRIT Feature, the QUANTAX EDS system's automated feature analysis module. Combining morphological and chemical classifi cation made it possible to display several monazite generations formed upon chemical weathering of carbonatites. High concentrations of La are shown in yellow, high concentrations of Nd in red, intermediate concentrations of La and Nd in blue and cerianite is shown in green.

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A new definition of µ-XRF

25 Megapixel Element Map of Concrete
25 megapixel element map of a concrete
sample, produced with the M4 TORNADO

The image shows the distribution of elements in a concrete sample. Red represents Al, green Si, blue Ca, turquoise Fe and pink Ti. Pores in the sample are black, as they don't contribute to the measurement signal. The 25 megapixel element map of the 10x10 cm2 sample was acquired using an M4 TORNADO μ-XRF spectrometer with a polycapillary lens under low vacuum conditions at 50 kV, 600 μA. Prior to acquisition, sample preparation was limited to rough polishing.

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Advanced Phase-ID

Demonstrating Advanced Phase-ID on a Mineral Sample
Demonstrating Advanced Phase-ID on
a mineral sample. Ten different phases
could be determined

The image above shows the phase distribution in a mineral sample. It contains ten
different phases representing all crystal symmetries from triclinic to cubic. The Kikuchi pattern and the EDS spectrum corresponding to an ilmenite particle (green) are also presented. The new bruker Advanced Phase-ID feauture was used to determine the phases. The shown results are courtesy of Dr. Angela Halfpenny from CSIRO in Perth, Australia.

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From micro- to nano-scale in a single map

12 Megapixel Map of an Oceanic Drill Core
12 megapixel map of an oceanic drill core

Element maps within minutes using the QUANTAX EDS system with XFlash® SDD: The complex matrix of this lower impact melt breccia at the Yaxcopoil-1 drill core (Unit 5 at 861.72 m) of the Chicxulub impact crater is dominated by Mg-rich clays (blue) and calcite (magenta) and contains partially resorbed andradite garnet [Ca3(Fe3+,Ti)2Si3O12, pink], interpreted to have formed from a hydrothermal fluid (Salge & Newsom, 2010). Sample courtesy International Continental Scientific Drilling Program and Natural History Museum, Berlin, Germany.

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Read more about the analysis of the drill core sample described in our ad