Analytical Instrument Documents

Typical electron spin resonance (ESR) spectrometer uses a microwave resonator, which is usually called a cavity, as a sensitive detector. A sample is usually set in the center of the cavity, and energy absorption by ESR phenomena is detected according to the degree of an impedance mismatching of the resonant circuit of the cavity. Absorption intensity in the ESR and FMR (Ferromagnetic Resonance) is proportional to the square root of the irradiated microwave power and the spin amount in the measured sample. Moreover, the spectral line width is proportional to the inverse of the transverse relaxation time of spins. The cavity is a device that stores only the light, of which the frequency is 𝜔𝑐=2𝜋𝑓𝑐, in the limited space. Electron spins lied in a static magnetic field are like spinning tops which are locked to specific Larmor frequency (𝜔𝑟=2𝜋𝑓𝑟). ESR/FMR spectrum is usually measured in the condition of 𝜔𝑐=𝜔𝑟. Recently, many attentions are gathering to the interaction between light (microwave) and spins in the cavity according to the development of quantum optics.

Coupling constant (𝑔𝑚) between microwave photon and electron spins is proportional to the square root of spin numbers as shown in eq.(1) of "Application Note ER200007E ". Therefore, FMR measurements using ferromagnets which include many spins and especially have narrow line widths do not work well, because spins in ferromagnets interact strongly with microwave photon, and achieve to "strong coupling" state larger than the state of "Purcell effect". Figure 1(a) is an example that shows the obtained unexpected spectrum in the strong coupling state. Normal FMR spectrum can be obtained as shown in Fig.1(d), if the filling factor is reduced and the system moves to a "weak coupling" state.

Some of the characteristic compounds that are responsible for the bright colors of autumn leaves are readily detected by using various ambient ionization methods with the AccuTOF-DART mass spectrometer system.

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.


Other Resources

Image Gallery
  • View a selection of NMR and MS spectra
  • Walkup NMR
  • See how the Delta NMR software allows users to just "walk up" and start NMR experiments
  • Mass Spec Reference Data
  • View our page of useful molecular references for Mass Spec
  • Tutorials (Mass Spec)
  • Documents on the basics of mass spectrometry
  • Delta NMR software Tutorials
  • Videos on how to use the Delta NMR software
  • No-D NMR
  • Description of No-D NMR and how it can be used to eliminate the need for deuterated solvents
  • Non Uniform Sampling (NUS)
  • Description of how NUS is used to greatly reduce the time needed for running NMR experiments
  • NMR Basics
  • Overview of the Basics of NMR Theory
  • NMR Magnet Destruction
  • See our presentation of the slicing open of a JEOL Delta-GSX 270 MHz NMR Magnet
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    January 28, 2022
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