Pulse sequence for time

Figure 8.4 Pulse sequence for time-resolved fluorescence measurement...

Fig. 2. The pulse sequence for the CP/MAS experiment. The values of the different time parameters depend on the relaxation behaviours and on the mobilities of the nuclei in the compounds investigated. (Reproduced with permission of Ref. I0))...

The INEPT experiment can be modified to allow the antiphase magnetization to be precessed for a further time period so that it comes into phase before data acquisition. The pulse sequence for the refocused INEPT experiment (Pegg et al., 1981b) is shown in Fig. 2.13. Another delay, A. is introduced and 180° pulses applied at the center of this delay simultaneously to both the H and the C nuclei. Decoupling during data acquisition allows the carbons to be recorded as singlets. The value of Z), is adjusted to enable the desired type of carbon atoms to be recorded. Thus, with D, set at V4J, the CH carbons are recorded at VsJ, the CH2 carbons are recorded and at VeJ, all protonated carbons are recorded. With D3 at %J, the CH and CH ( carbons appear out of phase from the CH2 carbons. 

Figure 5.7 (A) Pulse sequence for gated decoupled /-resolved spectroscopy. It involves decoupling only during the first half of the evolution period

Figure 6.2 Pulse sequences for some common 3D time-domain NMR techniques. Nonselective pulses are indicated by filled bars. Nonselective pulses of variable flip angle are shown by the flip angle )8. Frequency-selective pulses are drawn with diagonal lines in the bars. (Reprinted from J. Mag. Reson. 84, C. Griesinger, et al, 14, copyright (1989), with permission from Academic Press, Inc.)...

Fig. 2.9.2 Radiofrequency, field gradient and current distributions requires a three-dimen-ionic current pulse sequences for two-dimen- sional imaging sequence [see Figure 2.9.1(a)] sional current density mapping. TE is the Hahn and multiple experiments with the orientation spin-echo time, Tc is the total application time of the sample relative to the magnetic field of ionic currents through the sample. The 180°- incremented until a full 360°-revolution is pulse combined with the z gradient is slice reached. The polarity of the current pulses...

Figure 9 Timing diagram of the BIRD-HMBC pulse sequence for the detection of nJch correlations, including an additional two-step low-pass J filter. Thin and thick bars represent 90° and 180° pulses, respectively. 13C180° pulses are replaced by 90°y — 180°x — 90°y composite pulses. <5 is set to 0.5/(Vch) and A is set to 0.5/("JCH). Phases are cycled as follows fa = y, y, —y, —y 4>j = x, —x fa — 8(x), 8(—x) fa = 4(x), 4(— x) ( rec = 2 (x, — x), 4(—x, x), 2(x, —x). Phases not shown are along the x-axis. Gradient pulses are represented by filled half-ellipses denoted by Gi-G3. They should be applied in the ratio 50 30 40.1.

Fig. 5 Radio frequency pulse sequences for measurements of Sj and Si in DSQ-REDOR experiments. The MAS period rR is 100 ps. XY represents a train of 15N n pulses with XY-16 phase patterns [98]. TPPM represents two-pulse phase modulation [99]. In these experiments, M = Nt 4, N2+ N3 = 48, and N2 is incremented from 0 to 48 to produce effective dephasing times from 0 to 9.6 ms. Signals arising from intraresidue 15N-13C DSQ coherence (Si) are selected by standard phase cycling. Signal decay due to the pulse imperfection of 15N pulses is estimated by S2. Decay due to the intermolecular 15N-I3C dipole-dipole couplings is calculated as Si(N2)/S2(N2). The phase cycling scheme can be found in the original figure and caption. (Figure and caption adapted from [45])...

Fig. 8 Pulse sequence for the measurement of homonuclear correlation spectra with 7 filtering. Narrows bars indicate 7t/2 pulses and broad bars indicate 71 pulses. Experimental conditions employed for a-synuclein fibrils samples static field strength 9.4 T temperature —5 °C spinning frequency 8 kHz T2 filter 100 ms CP contact time 2.5 ms TOBSY mixing time 6 ms. The rf phases can be found in the original figure and caption. (Figure and caption adapted from the Supporting Information of [134]. Copyright (2005) National Academy of Sciences, USA)...

Fig. 21 HMQC pulse sequences for (a) 14N-13C and (b) 14N- H correlations under rotor-synchronized MAS. In (b), dipolar recoupling is usually applied during time intervals Texc and Trec. (c) Coherence transfer pathways for the observation of SQ (solid lines) and DQ (dashed lines) in the 14N dimension...

In addition to measuring TCH for the polymorphic system in question, the proton T value must be determined since the repetition rate of a CP experiment is dependent upon the recovery of the proton magnetization. Common convention states that a delay time between successive pulses of 1-5 X T, must be used. Figure 10B outlines the pulse sequence for measuring the proton Tx through the carbon intensity. One advantage to solids NMR work is that a common proton Tx value will be measured, since protons communicate through a spin-diffusion process. An example of spectral results obtained from this pulse sequence is displayed in Fig. 12. 

Fig. 11.7 a Pulse sequence for rotational-resonance recoupling of homonuclear spin pairs, b The spinning frequency is matched to the isotropic chemical-shift difference, and one of the resonances is selectively inverted and the polarization exchange measured as a function of the mixing time, c The difference polarization as a function of the mixing can be evaluated to give the dipolar coupling constant. 

Figure 5. The rf pulse sequences for determining SL cross polarization time constant Ten, C-13 T,p and C-13 Tj under proton decoupling. Each experiment starts with a SL cross polarization.

Pig. 1. Pulse sequence for selective reverse INEPT. The time-shared homonuclear decoupling during acquisition is optional, and a variety of simplifications may be made to the sequence depending on the instrument used and on the spin system under investigation, as discussed in the text. A DANTE sequence is shown as the selective 90° carbon-13 pulse, but this may be replaced by a soft pulse or some other form of selective excitation. Phase cycling for this sequence is summarized in table 1. 

Fig. 2. Pulse sequence for selective reverse INEPT using pulsed field gradients to select the coherence transfer echo. The 180° pulse pair in the middle of the 2r delay is not normally needed for t < 50 ms, and the second proton 180° pulse and first t2 delay maybe omitted if a linear phase gradient in the resultant spectrum can be tolerated. The second field gradient pulse has an area (7c/th) times that of the first.

Fig. 1. LED pulse sequence for the measurement of stimulated echoes attenuated by diffusion. Typical values for delays and pulse widths are 5 ms for the gradient pulse widths tg, 2-3 ms for the recovery time tr, 0.1 s for the diffusion time td, and 5 ms for the storage time...

Fig. 1. Pulse sequences for determining spin-lattice relaxation time constants. Thin bars represent tt/2 pulses and thick bars represent tt pulses, (a) The inversion-recovery sequence, (b) the INEPT-enhanced inversion recovery, (c) a two-dimensional proton-detected INEPT-enhanced sequence and (d) the CREPE sequence. T is the waiting period between individual scans. In (b) and (c), A is set to (1 /4) Jm and A is set to (1 /4) Jm to maximize the intensity of IH heteronuclei and to (1/8) Jm to maximize the intensity of IH2 spins. The phase cycling in (c) is as follows 4>i = 8(j/),8(-j/) 3 = -y,y A = 2(x),2(-x) Acq = X, 2 —x), X, —X, 2(x), —x, —x, 2(x), —x, x, 2 —x),x. The one-dimensional version of the proton-detected experiment can be obtained by omitting the f delay. In sequence (d), the phase 4> is chosen as increments of 27r/16 in a series of 16 experiments.

The development of carbon-13 NMR during the last eight years has been characterized by a continual increase in the sensitivity and quality of spectra. A reduction in measuring time - equivalent to an enhancement in sensitivity has been achieved mainly by cryomagnet technology. The efficiency with which NMR information can be obtained has been substantially improved by new computer-controllable pulse sequences for one-and two-dimensional NMR experiments. A selection of these new methods, in particular, those used for multiplicity analysis and homo- or heteronuclear shift correlations, is presented in chapter 2 of this edition. 

Fig. 83. Pulse sequence for the 2D SLF spectrum of 1 JC- H interactions (414). During evolution period, r, mainly heteronuclear spin interactions are effective, whereas chemical shift interactions govern the time evolution during the detection period, r2 (see text).

Heterocorrelations can be detected both in direct and reverse modes. In the latter mode, dramatic enhancements of sensitivity can be achieved owing to the larger sensitivity of protons with respect to heteronuclei. In the most common heterocorrelation pulse sequences for reverse detection, called heteronuclear multiple quantum coherence (HMQC) (Fig. 8.2G) [25,26], H-I3C MQ (multiple quantum) coherence is generated by first applying a 90° pulse on protons and, after a time t chosen equal to 1/2 J[j, by applying a 90° pulse on carbon (Fig. 8.19). 

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