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1.
Microsc Microanal ; 24(6): 657-666, 2018 12.
Article in English | MEDLINE | ID: mdl-30523773

ABSTRACT

We present a flexible linear optimization model for correcting multi-angle curtaining effects in plasma focused ion beam scanning electron microscopy (PFIB-SEM) images produced by rocking-polishing schemes. When PFIB-SEM is employed in a serial sectioning tomography workow, it is capable of imaging large three-dimensional volumes quickly, providing rich information in the critical 10-100 nm feature length scale. During tomogram acquisition, a "rocking polish" is often used to reduce straight-line "curtaining" gradations in the milled sample surface. While this mitigation scheme is effective for deep curtains, it leaves shallower line artifacts at two discretized angles. Segmentation and other automated processing of the image set requires that these artifacts be corrected for accurate microstructural quantification. Our work details a new Fourier-based linear optimization model for correcting curtaining artifacts by targeting curtains at two discrete angles. We demonstrate its capabilities by processing images from a tomogram from a multiphase, heterogeneous concrete sample. We present methods for selecting the parameters which meet the user's goals most appropriately. Compared to previous works, we show that our model provides effective multi-angle curtain correction without introducing artifacts into the image, modifying non-curtain structures or causing changes to the contrast of voids. Our algorithm can be easily parallelized to take advantage of multi-core hardware.

2.
Magn Reson Chem ; 48(8): 630-41, 2010 Aug.
Article in English | MEDLINE | ID: mdl-20589732

ABSTRACT

The INADEQUATE experiment can provide unequalled, detailed information about the carbon skeleton of an organic molecule. However, it also has the reputation of requiring unreasonable amounts of sample. Modern spectrometers and probes have mitigated this problem, and it is now possible to get good structural data on a few milligrams of a typical organic small molecule. In this paper, we analyze the experiment step by step in some detail, to show how each part of the sequence can both contribute to maximum overall sensitivity and can lead to artifacts. We illustrate these methods on three molecules: 1-octanol, the steroid 17alpha-ethynylestradiol and the isoquinoline alkaloid beta-hydrastine. In particular, we show that not only is the standard experiment powerful, but also a version tuned to small couplings can contribute vital structural information on long-range connectivities. If the delay in the spin echo is long, pairs of carbons with small couplings can create significant double-quantum coherence and show correlations in the spectrum. These are two- and three-bond correlations in a carbon chain or through a heteroatom in the molecule. All these mean that INADEQUATE can play a viable and important role in routine organic structure determination.


Subject(s)
1-Octanol/chemistry , Benzylisoquinolines/chemistry , Ethinyl Estradiol/chemistry , Ethinyl Estradiol/analogs & derivatives , Magnetic Resonance Spectroscopy/standards , Molecular Structure , Reference Standards
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