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This study focuses on the evaluation of the crystal structure perfection in the single crystal made of CMSX-4 nickel superalloy and its effect on creep resistance. Single crystal castings were manufactured by directional solidification process at the withdrawal rate of 1, 3, 5 and 7 mm/min. Light (LM) and electron (SEM, TEM) microscopy, X-ray diffraction and Mossbauer spectroscopy were used for evaluation of the microstructure and crystal structure perfection. Castings were also subjected to creep tests. The best creep resistance was obtained for the casting manufactured at the withdrawal rate of 3 mm/min, characterized by the highest crystal structure perfection compared to the other castings examined. [ABSTRACT FROM AUTHOR]

A new generation of microscale, nuclear magnetic resonance (CapNMR) probe technology employs two independent detection elements to accommodate two samples simultaneously. Each detection element in the dual-sample CapNMR probe (DSP) delivers the same spectral resolution and S/N as in a CapNMR probe configured to accommodate one sample at a time. A high degree of electrical isolation allows the DSP to be used in a variety of data acquisition modes. Both samples are shimmed simultaneously to achieve high spectral resolution for simultaneous data acquisition, or alternatively, a flowcell-specific shim set is readily called via spectrometer subroutines to enable acquisition from one sample while the other is being loaded. An automation system accommodates loading of two samples via dual injection ports on an autosampler and two completely independent flowpaths leading to dedicated flowcells in the DSP probe.

A microflow CapNMR probe double-tuned for 1H and 13C was installed on a 400-MHz NMR spectrometer and interfaced to an automated liquid handler. Individual samples dissolved in DMSO-d6 are submitted for NMR analysis in vials containing as little as 10 microL of sample. Sets of samples are submitted in a low-volume 384-well plate. Of the 10 microL of sample per well, as with vials, 5 microL is injected into the microflow NMR probe for analysis. For quality control of chemical libraries, 1D NMR spectra are acquired under full automation from 384-well plates on as many as 130 compounds within 24 h using 128 scans per spectrum and a sample-to-sample cycle time of approximately 11 min. Because of the low volume requirements and high mass sensitivity of the microflow NMR system, 30 nmol of a typical small molecule is sufficient to obtain high-quality, well-resolved, 1D proton or 2D COSY NMR spectra in approximately 6 or 20 min of data acquisition time per experiment, respectively. Implementation of pulse programs with automated solvent peak identification and suppression allow for reliable data collection, even for samples submitted in fully protonated DMSO. The automated microflow NMR system is controlled and monitored using web-based software.