Analytical Instrument Documents

Diffusion-ordered spectroscopy (DOSY) is a powerful NMR method for the analysis of mixtures. In DOSY, signals in the NMR spectrum are resolved according to the measured diffusion coefficient for each signal, yielding a 2D spectrum which has chemical shift along the x-axis and diffusion coefficient along the y-axis.

NOE (Nuclear Overhauser Effect) correlations  comprise important information to estimate internuclear distance and determine structure. However, NOE correlation peaks are very weak compared with diagonal peaks in 2D NOESY. For this reason, it is difficult to observe NOE correlation peaks in the vicinity of much larger diagonal peaks.

The ROYALPROBE™ HFX can simultaneously irradiate 1H, 19F, and 13C (or other X-nuclei) even in a basic console with basic two-channel console, and is a versatile probe that can measure a wide-variety of nuclei at high sensitivity. Here we introduce some useful experiments for fluorine-containing compounds that can be run on conjunction with JNM-ECZ400S equipped with ROYALPROBE™ HFX.

1H, in principle, is very useful nucleus to investigate atomic-resolution structures and dynamics due to its high abundance (>99%) and gyromagnetic ratio (600 MHz at 14.1T). In fact 1H is the first choice of nucleus in solution NMR. On the other hand, 1H NMR of rigid solids is much less common. This is because 1H solid-state NMR gives very broad (~50 kHz) and featureless spectra (Fig 1a) due to strong 1H-1H dipolar coupling, which is dynamically averaged out in solution. Magic angle spinning (MAS) removes the broadening to the first order, but is not enough to achieve high resolution 1H NMR at moderate MAS rate (Fig 1b). Tremendous efforts were made to overcome this issue from the early dates of solid-state NMR towards high-resolution 1H NMR [1]. Most of them combine MAS with sophisticated 1H pulses which is dubbed CRAMPS (combined rotation and multiple pulse spectroscopy). Nowadays very fast MAS > 60 kHz can be used to achieve high-resolution 1H solid-state NMR (Fig 1c) [2]. However, the traditional CRAMPS is still useful as that can be performed with very conventional solid-state NMR equipment, for example 4 mm MAS probe with a 400 MHz spectrometer. Moreover, wPMLG at moderate MAS rate often overwhelms fast MAS in terms of resolution. In this note, we will describe tutorial guidance to optimize experimental parameters for CRAMPS.

Multidimensional correlation NMR spectroscopies, which provides inter-nuclear proximity/connectivity, play a crucial role to probe the atomic resolution structures. Especially, 1H-1H homonuclear correlation spectroscopy is quite useful source of information because of high abundance (>99%) and gyromagnetic ratio, thus resulting in strong inter nuclear interactions. Thanks to the development of high resolution 1H solid-state NMR, now it is feasible to observe 1H-1H correlation high resolution solid-state NMR [1]. There are two distinctive categories; 1) single quantum (SQ)/SQ correlation and 2) double quantum (DQ)/SQ correlations. In this note we introduce 2D 1H SQ/ 1H SQ and 1H DQ/ 1H SQ correlation spectroscopy to probe the internuclear proximity using high-resolution 1H solid-state NMR techniques.

The JMS-T200GC  AccuTOF™ GCx-plus is a superior gas chromatograph - high-resolution time-of-flight mass spectrometer (GC-HRTOFMS) system that simultaneously accomplishes high mass-resolution analysis, high mass accuracy, and high-speed data acquisition, satisfying all your needs for petroleum and petrochemical analyses.

Field Desorption (FD) is a technique that ionizes analytes by electron tunneling from the analyte molecules to a solid surface (emitter) in a high electric field. The sample is applied directly onto the emitter and heated by applying an electric current through the emitter for desorption and ionization. FD has been used for the analysis of nonvolatile compounds, synthetic polymers, etc., as a soft ionization method to produce molecular ions with little or no fragmentations. As a result, the average molecular weight of a sample can be calculated directly from the masses (or “m/z”) and intensities for all of the ions observed in the FD mass spectrum. Furthermore, by applying group-type analysis, the components can be classified into types based on their functional groups and/or unsaturations. Average molecular weight, polydispersity index, or relative abundance of each type can also be obtained. In this work, new and used rotary vacuum pump (RP hereafter) oils were analyzed by FD. Afterwards, the change in their compositions was determined by performing group-type analysis on the resulting mass spectra.

Among the various methods used for characterizing plastics, pyrolysis (Py) GC/MS and thermal desorption (TD) GC/MS are widely used for both qualitative and quantitative analyses. These are simple techniques that provide detailed information about the samples. In this application note, we report the analysis of additives in plastic by using a thermal desorption system and a JEOL JMS-T100GCV "AccuTOF GCv" GC-TOFMS. Identification of the analytes was accomplished by library search and accurate mass measurement. Additionally, isotope cluster pattern matching was performed using the "Mass Spec Tools™" software to help identify an unknown compound that was present in the sample.

Lithium ion secondary batteries using spinel-type lithium titanium oxide (LTO) as the negative electrode material are excellent in safety and cycle characteristics due to their chemical stability, and have already been put into practical use.

The ESR Spectrometer JES-X3 series has an improved low-noise Gunn oscillator, providing a 30% improvement in sensitivity compared to previous models. ESR is the only instrument for directly detecting paramagnetic species. This supports a variety of applications in research, development, inspection and evaluation.