Spatially resolved Gd, Fe, and Mn concentrations were determined with LA-ICP-MS for specific quantitative analysis of metal content within the DCN and GP region. One hemisphere was embedded in Tissue Tek O.C.T. Compound (Sakura Finetek; Alphen aan den Rijn, the Netherlands) directly after extraction and snap frozen with isopentane. The tissue was cryosectioned in 10 μm thin coronal slices and mounted on Superfrost Ultra Plus adhesive glass slides (Menzel Glaeser, Braunschweig, Germany). Laser ablation was performed with an inductively coupled plasma mass spectrometer (Thermo iCap RQ ICP-MS, Thermo Fisher Scientific, Waltham, MA) coupled to a laser ablation system (ESI NWR 213; New Wave Research, Fremont, CA), as previously described.19 (link),54 (link) Images were generated, and the elements were identified with ImaJar software (kindly provided by Robin Schmid and Uwe Karst, University of Muenster, Germany). Gelatin standards containing known Mn/Fe/Gd concentrations were sliced in the same way as the tissue and measured in each session for calibration and quantification in tissue samples. Regions of interest were localized and drawn on the Fe/Mn images around the DCN and the GP for local quantification and statistics.
Thermo icap rq icp ms
Manufactured by Thermo Fisher Scientific
The Thermo iCap RQ ICP-MS is an inductively coupled plasma mass spectrometer. It is designed for the analysis of trace elements in a variety of sample types.
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2 protocols using thermo icap rq icp ms
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Spatially Resolved Metal Analysis of DCN and GP
2
Multilayer LLTO and LCO Thin Film Composition
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The multilayer sample used in this study was composed of four repeating units of LLTO and LCO layers grown by pulsed-laser deposition on Si(100). Using X-ray photoelectron spectroscopy (XPS), it was determined that the top layer exhibited a composition of Li0.09La0.64TiO3. However, because XPS has poor sensitivity to Li and small errors in La:Ti ratios yield large errors in Li concentration estimates, a more accurate test of composition was performed. The films were digested with aqua regia solution for 3 days to ensure complete dissolution. The resulting supernatant was diluted with 3% HNO3 for analysis by inductively coupled plasma mass spectrometry (ICP–MS). All measurements used either Thermo iCAP Q ICP–MS or Thermo iCAP RQ ICP–MS. This resulted in a stoichiometry of Li0.41Li0.53TiO3 (see Supplementary Section 3 for XPS and ICP–MS measurements and additional discussion). The top layer is LLTO, which is ~11 nm in thickness. See Supplementary Fig. 4 for hard X-ray reflectivity measurements that enabled determination of the layer structure represented in the inset of Fig. 1c . Densities were determined by neutron reflection (Supplementary Fig. 5 ).
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