Unique Usage of a Classical Selective Homodecoupling Sequence for High-Resolution Quantitative 1H NMR.

Classical selective homodecoupling was used in a 1H NMR purity assay to improve accuracy by overcoming spectral overlaps due to 1H-1H spin coupling. Dummy irradiation at a specific frequency was used in addition to irradiation at a 1H resonance of the analyte to avoid irradiation bias. The method was validated in a 1H NMR purity assay of high-purity diethyl phthalate (National Metrology Institute of Japan Certified Reference Material (NMIJ CRM), purity: 99.98%). The obtained purity value biases were 0.27% or less. The utility of the method was demonstrated in another 1H NMR purity assay of dipropyl phthalate (NMIJ CRM, purity: 98.41%), which contained a tiny amount of the structurally similar compound methyl propyl phthalate as an impurity. An accurate assay was achieved with the method, giving a purity of 98.39%, whereas the conventional method gave a purity 99.13%.

24 T High-Resolution and -Sensitivity Solid-State NMR Measurements of Low-Gamma Half-Integer Quadrupolar Nuclei 35Cl and 37Cl.

Solid-state NMR observations of low-gamma half-integer quadrupolar nuclei, 35Cl and 37Cl, were demonstrated using a 24 T hybrid magnet (1H resonance frequency of 1.02 GHz) comprised of the high-temperature (HTS) and low-temperature (LTS) superconductors, and compared with results using a 14.1 T standard NMR magnet. While at 24 T the linewidth is 1.7 times narrower than that at 14.1 T, the gain in the sensitivity is 7.0 times because of enhanced polarization, reduced linewidth, and the use of larger rotor. A simple theoretical model was used to rationalize the sensitivity enhancements. The ratio of 35Cl and 37Cl quadrupolar couplings agrees well with the ratio of quadrupolar moments, and no isotope-dependent chemical shift has been observed. In addition, the 3QMAS spectrum of 35Cl is shown to demonstrate the high sensitivity rendered by the 24 T spectrometer.

The application of phenylmethanethiol and benzenethiol derivatives as odorless organosulfur reagents in the synthesis of thiosugars and thioglycosides.

p-octyloxyphenylmethanethiol and p-dodecylbenzenethiol were prepared as new odorless organosulfur reagents. Thiosugars and thioglycosides were synthesized using these reagents without encountering any malodorous procedures.

1020MHz single-channel proton fast magic angle spinning solid-state NMR spectroscopy.

This study reports a first successful demonstration of a single channel proton 3D and 2D high-throughput ultrafast magic angle spinning (MAS) solid-state NMR techniques in an ultra-high magnetic field (1020MHz) NMR spectrometer comprised of HTS/LTS magnet. High spectral resolution is well demonstrated.

One step polymerizing technique for fabricating a hollow obturator.

PURPOSE: Although a closed hollow obturator is often applied to post maxillectomy patients, it has a few problems such as complexity of fabrication and water leakage to inside. A one step curing technique to fabricate a closed hollow obturator by constructing a small hollow bulb made by two thermoplastic resin sheets is described in the present report. METHODS: In the one step curing technique, after dewaxing the wax denture fabricated conventionally, one size smaller hollow body was fabricated with two thermoplastic resin sheets and set into the investment mold as a core. Then the circumferential part of obturator was cured by the pour type resin. This technique was used to fabricate an obturator prosthesis in a 60-year-old post-maxillectomy patient. The weight of this obturator was well controlled and the definitive prosthesis weighed 22 g. At a one year follow-up, the obturator fared well without any water leakage or breakage. CONCLUSIONS: This technique allows the fabricator to control the thickness and weight of the obturator by the amount of relief provided by the hollow bulb. It also rectifies the disadvantages of the closed hollow obturator such as water leakage and complexity of fabrication.