Inversion pulse sequence

XCOR Spectra. A recent improvement made in 2D-heteronu-clear correlated spectroscopy is the use of a selective proton inversion pulse sequence which increases the sensitivity of the experiment by removing proton homonuclear coupling and allows easier correlation between and chemical shifts. The XCOR pulse sequence used for the purpose is shown in... 

Figure Bl.14.9. Imaging pulse sequence including flow and/or diflfiision encoding. Gradient pulses before and after the inversion pulse are supplemented in any of the spatial dimensions of the standard spin-echo imaging sequence. Motion weighting is achieved by switching a strong gradient pulse pair G, (see solid black line). The steady-state distribution of flow (coherent motion) as well as diffusion (spatially...

The values of the time constants and are important in understanding both internal and overall motional behavior of the sample molecule. values are measured by the inversion recovery pulse sequence ... 

HC HMQC (heteronuclear multiple quantum coherence) and HC HSQC (heteronuclear single quantum coherence) are the acronyms of the pulse sequences used for inverse carbon-proton shift correlations. These sensitive inverse experiments detect one-bond carbon-proton connectivities within some minutes instead of some hours as required for CH COSY as demonstrated by an HC HSQC experiment with a-pinene in Fig. 2.15. 

HSQC Heteronuclear single quantum coherence, e.g. inverse CH correlation via one-bond coupling providing the same result as HMQC but using an alternative pulse sequence... 

The most popular, and also a very accurate, experimental method for measuring nonselective spin-lattice relaxation-rates is the inversion recovery (180°-r-90°-AT-PD)NT pulse sequence. Here, t is the variable parameter, the little t between pulses, AT is the acquisition time, PD is the pulse delay, set such that AT-I- PD s 5 x T, and NT is the total number of transients required for an acceptable signal-to-noise ratio. Sequential application of a series of two-pulse sequences, each using a different pulsespacing, t, gives a series of partially relaxed spectra. Values of Rj can... 

Fig. 1.—Diagrammatic Representation of the Recovery of Magnetization along the z-Axis (Mj), from Its Initial Value (-M ) to +Mo, Following Its Inversion by a 180° Pulse. The exponential recovery curve shown in [A] depicts the return of magnetization that would be found in a typical inversion-recovery experiment. The curve in [B] would be obtained from a three-pulse sequence, and is a plot of which decreases from an initial value of...

It is important to avoid saturation of the signal during pulse width calibration. The Bloch equations predict that a delay of 5 1] will be required for complete restoration to the equilibrium state. It is therefore advisable to determine the 1] values an approximate determination may be made quickly by using the inversion-recovery sequence (see next paragraph). The protons of the sample on which the pulse widths are being determined should have relaxation times of less than a second, to avoid unnecessary delays in pulse width calibration. If the sample has protons with longer relaxation times, then it may be advisable to add a small quantity of a relaxation reagent, such as Cr(acac) or Gkl(FOD)3, to induce the nuclei to relax more quickly. 

Figure 2.9 Pulse sequence for the INEPT experiment. (B) Effect of pulses on H magnetization. Application of the pulse sequence shown results in population inversion of one of the two proton vectors of the CH doublet and therefore causes an intensification of the corresponding C lines.

F ure 2.16 Pulse sequence for the inverse (reverse) DEPT experiment. 

The SELINCOR experiment is a selective ID inverse heteronuclear shift-correlation experiment i.e., ID H,C-COSYinverse experiment) (Berger, 1989). The last C pulse of the HMQC experiment is in this case substituted by a selective 90° Gaussian pulse. Thus the soft pulse is used for coherence transfer and not for excitation at the beginning of the sequence, as is usual for other pulse sequences. The BIRD pulse and the A-i delay are optimized to suppress protons bound to nuclei As is adjusted to correspond to the direct H,C couplings. The soft pulse at the end of the pulse sequence (Fig. 7.8) serves to transfer the heteronuclear double-quantum coherence into the antiphase magnetization of the protons attached to the selectively excited C nuclei. 

Figure 7.8 SELINCOR (Selective Inverse Correlation) pulse sequence with BIRD presaturation. (Reprinted from Mag. Reson. Chem. 29, H, Kessler et ai, 527, copyright (1991), with permission from John Wiley and Sons Limited, Baffins Lane, Chichester, Sussex P019 lUD, England.)...

Inversion recovery A pulse sequence used to determine spin-lattice relaxation times. 

Fig. 1.19 Spin-echo based pulse sequence to each gradient pulse, A the separation between encode velocity change. The gradients are each pair of bipolar gradient pulses and tm the stepped pair-wise independently (2D VEXSY) mixing time between the bipolar gradient pairs, or simultaneously (1 D VEXSY). For a VEXSY The opposite polarity of the bipolar gradient experiment, 7q to k4 are usually applied along pair is realized by an inversion 180° pulse, the same spatial direction. 8 is the duration of...

The idea of exploration of relaxation correlation was first reported in 1981 by Peemoeller et al. [23] and later by English et al. [24] using an inversion-recovery experiment detected by a CPMG pulse train. This pulse sequence is shown in Figure 2.7.1. 

NMR interpretation has made significant advances with diffusion-editing pulse sequences and two-dimensional inversion of diffusivity and T2 relaxation [7,40-44]. The 2D inversion can also be used to compare Tj and T2 relaxation with each other [42]. Distributions of these two characteristic parameters can now be displayed on a 2D map and the relationship between them more easily visually interpreted. The 2D distribution map can be interpreted by comparing the measured distribution with the line for the bulk diffusivity of water and the correlation lines for the hydrocarbon components in crude oils, shown in Figure 3.6.10 as dashed lines [40-46]. Figure... 

T, values can be easily determined using pulse sequences which form part of the standard computer software, the most common one being the so-called inversion-recovery experiment. 

Fig. 9 Spectra of compound 1 obtained from an inversion-recovery experiment. Pulse sequence fixed delay - 180° pulse - variable delay x - 90° pulse - acquisition of FID...

Fig. 2 (a) DRAMA pulse sequence (using % = t/2 = rr/4 in the text) and a representative calculated dipolar recoupled frequency domain spectrum (reproduced from [23] with permission), (b) RFDR pulse sequence inserted as mixing block in a 2D 13C-13C chemical shift correlation experiment, along with an experimental spectrum of 13C-labeled alanine (reproduced from [24] with permission), (c) Rotational resonance inversion sequence along with an n = 3 rotational resonance differential dephasing curve for 13C-labeled alanine (reproduced from [21] with permission), (d) Double-quantum HORROR experiment along with a 2D HORROR nutation spectrum of 13C2-2,3-L-alanine (reproduced from [26] with permission)... 

Siegel et al. showed that enhancement of the CT can also be obtained using hyperbolic secant (HS) pulses to invert selectively the STs [74], Unlike the DFS waveform, whose frequency sweep is generated by a constant rf-pulse phase while modulating the amplitude, the HS pulse utilizes both amplitude and phase modulation, yielding an enhancement exceeding that obtained by DFS or RAPT [61, 74, 75]. Most recently, the pulse sequence called wideband uniform-rate smooth truncation (WURST) [76] was introduced to achieve selective adiabatic inversion using a lower power of the rf-field than that required for the HS pulses [77,78]. One of its applications involved more efficient detection of insensitive nuclei, such as 33S [79]. 

This effect induces a free induction decay (FID) signal in the detection circuit. The FID can be measured, and the normal absorption spectrum can be obtained by means of an inverse Fourier transform. A variety of experimental extensions have been developed for this approach. By means of particular pulse sequences it is possible to detect spin resonances selectively on the basis of a broad ensemble of properties such as spatial proximity and dipolar coupling strengths. The central fundamental quantity of interest is, however, still the energy spectrum of the nuclear spin,... 

Because the excitation/detection coil is in the x-y plane and the longitudinal component relaxes along the z axis, T cannot be measured directly from an NMR spectrum, but must be obtained using a pulse sequence. The most commonly used pulse sequence to measure T is an inversion recovery pulse sequence (Kemp, 1986). Other commonly used pulse sequences for measuring 7j are given in Ernst et al. (1987). 

A number of pulse-sequence methods are available for measurement of Ti values, and those most commonly used are the methods of saturation recovery (s.r.F.t.),69,70 progressive saturation (p.s.F.t.),71 inversion recovery (i.r.F.t.),72 and the Freeman-Hill modification of in-... 

FIGURE 31. Typical data set for measurement of the spin-lattice relaxation times of the sp2-hybridized carbon atoms of, 6-carotene at 11.7 T. The chemical shift values are shown across the bottom of the figure. The t-value for each spectrum is the delay time in the inversion-recovery pulse sequence. Reprinted with permission from Reference 49. Copyright (1995) American Chemical Society... 

Figure 10.7 Carr-Purcell-Meiboom Gill (CPMC) sequence and NMR signal. (A) CPMC pulse sequence, (B) CPMC decay signal, and (C) Laplace inversion of the CPMC decay signal.

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