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Title: Advanced tomography techniques for inorganic, organic, and biological materials



Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
OSTI Identifier:
Report Number(s):
Journal ID: ISSN 0883-7694; KP1606000
DOE Contract Number:
Resource Type:
Journal Article
Resource Relation:
Journal Name: MRS Bulletin; Journal Volume: 41; Journal Issue: 07
Country of Publication:
United States
transmission electron microscopy (TEM); scanning transmission electron microscopy (STEM); x-ray tomography

Citation Formats

Evans, James E., and Friedrich, Heiner. Advanced tomography techniques for inorganic, organic, and biological materials. United States: N. p., 2016. Web. doi:10.1557/mrs.2016.134.
Evans, James E., & Friedrich, Heiner. Advanced tomography techniques for inorganic, organic, and biological materials. United States. doi:10.1557/mrs.2016.134.
Evans, James E., and Friedrich, Heiner. 2016. "Advanced tomography techniques for inorganic, organic, and biological materials". United States. doi:10.1557/mrs.2016.134.
title = {Advanced tomography techniques for inorganic, organic, and biological materials},
author = {Evans, James E. and Friedrich, Heiner},
abstractNote = {Abstract},
doi = {10.1557/mrs.2016.134},
journal = {MRS Bulletin},
number = 07,
volume = 41,
place = {United States},
year = 2016,
month = 7
  • A procedure for determination of both organic and inorganic mercury in biological materials by graphite furnace atomic absorption spectrometry (GFAAS) is described. Organic mercury is extracted as a chloride derivative by benzene and reextracted by a thiosulfate solution. Inorganic mercury is converted into a methyl chloride derivative by methanolic tetramethyltin prior to extraction. A aliquot of the thiosulfate solution is injected into the graphite furnace. The calibration is linear up to 12 ng of Hg/20 injected. The limit of detection of mercury is 0.04 ng of Hg/20 injected. The organic mercury thiosulfate extract was treated with CuCl/submore » 2/, reextracted in the benzene layer, and analyzed by gas chromatography (GLC) for speciation.« less
  • We demonstrate the applications of several novel techniques in solid-state nuclear magnetic resonance spectroscopy (SSNMR) to the structural studies of mesoporous organic-inorganic hybrid catalytic materials. Most of these latest capabilities of solid-state NMR were made possible by combining fast magic angle spinning (at {ge} 40 kHz) with new multiple RF pulse sequences. Remarkable gains in sensitivity have been achieved in heteronuclear correlation (HETCOR) spectroscopy through the detection of high-{gamma} ({sup 1}H) rather than low-{gamma} (e.g., {sup 13}C, {sup 15}N) nuclei. This so-called indirect detection technique can yield through-space 2D {sup 13}C-{sup 1}H HETCOR spectra of surface species under natural abundancemore » within minutes, a result that earlier has been out of reach. The {sup 15}N-{sup 1}H correlation spectra of species bound to a surface can now be acquired, also without isotope enrichment. The first indirectly detected through-bond 2D {sup 13}C-{sup 1}H spectra of solid samples are shown, as well. In the case of 1D and 2D {sup 29}Si NMR, the possibility of generating multiple Carr-Purcell-Meiboom-Gill (CPMG) echoes during data acquisition offered time savings by a factor of ten to one hundred. Examples of the studied materials involve mesoporous silica and mixed oxide nanoparticles functionalized with various types of organic groups, where solid-state NMR provides the definitive characterization.« less
  • An atomic absorption procedure is described. The method determines total mercury and, selectively, inorganic mercury. Levels of mercury (7 ng Hg/ml) in whole blood of unexposed people can be determined with the following precision: total mercury 4.1%, inorganic mercury, 8.7% and organic mercury 5.6%. The atomic absorption detector was an LDC Mercury Monitor, Model 1235. 1 figure. (DP)