Distortionless enhancement of polarization transfer

Major advances m NMR have been made by using a second rf transmitter to irra diate the sample at some point during the sequence There are several such techniques of which we 11 describe just one called distortionless enhancement of polarization transfer, abbreviated as DEPT... 

DEPT (Section 13.18) Abbreviation for distortionless enhancement of polarization transfer. DEPT is an NMR technique that reveals the number of hydrogens directly attached to a carbon responsible for a particular signal. 

Figure 13.6 is the proton-decoupled carbon-13 NMR distortionless enhancement of polarization transfer (DEPT) spectra of poly(methyl-l-pentene) [29]. This experiment, after data manipulation, separates the methine, methylene, and... 

The complete PMR and C assignments for a series of differently substituted thiadiazin-2//-thiones 30-32, having different groups on the two heterocyclic nitrogen atoms, have been presented <2001MRC222>. To assign all of the NMR signals unequivocally, 1-D and 2-D techniques such as distortionless enhancement of polarization transfer (DEPT 135), heteronuclear multiple quantum correlation (HMQC), and heteronuclear multiple bond... 

Nuclear Magnetic Resonance Spectroscopy. Like IR spectroscopy, NMR spectroscopy requires little sample preparation, and provides extremely detailed information on the composition of many resins. The only limitation is that the sample must be soluble in a deuterated solvent (e.g., deuterated chloroform, tetrahydro-furan, dimethylformamide). Commercial pulse Fourier transform NMR spectrometers with superconducting magnets (field strength 4-14 Tesla) allow routine measurement of high-resolution H- and C-NMR spectra. Two-dimensional NMR techniques and other multipulse techniques (e.g., distortionless enhancement of polarization transfer, DEPT) can also be used [10.16]. These methods are employed to analyze complicated structures. C-NMR spectroscopy is particularly suitable for the qualitative analysis of individual resins in binders, quantiative evaluations are more readily obtained by H-NMR spectroscopy. Comprehensive information on NMR measurements and the assignment of the resonance lines are given in the literature, e.g., for branched polyesters [10.17], alkyd resins [10.18], polyacrylates [10.19], polyurethane elastomers [10.20], fatty acids [10.21], cycloaliphatic diisocyanates [10.22], and epoxy resins [10.23]. 

Techniques developed in recent years make it possible to obtain large amounts of information from l3C NMR spectra. For example, DEPT-NMR, for distortionless enhancement by polarization transfer, allows us to determine the number of hydrogens attached to each carbon in a molecule. 

Population transfer experiments may be selective or nonselective. Selective population transfer experiments have found only limited use for signal multiplicity assignments (SSrensen et al, 1974) or for determining signs of coupling constants (Chalmers et al., 1974 Pachler and Wessels, 1973), since this is better done by employing distortionless enhancement by polarization transfer (DEPT) or Correlated Spectroscopy (COSY) experiments. However, nonselective population transfer experiments, such as INEPT or DEPT (presented later) have found wide application. 

The most widely used method for determining multiplicities of carbon atoms is DEPT (Distortionless Enhancement by Polarization Transfer). This has generally replaced the classical method of recording off-resonance C spectra with reduced CH couplings from which the multiplicity could be read directly. 

You may be told that your NMR laboratory does not routinely use APT spectra but provides DEPT spectra (Distortionless Enhancement by Polarization Transfer) instead. This is no problem, as DEPT spectra also provide you with the information you need just go back and read what we have said about the relative merits of APT and DEPT. 

The first of these tools is the distortionless enhancement by polarization transfer (DEPT) pulse sequence. There are a number of versions of this experiment which can be very useful for distinguishing the different types of carbons within a molecule. Of these, we have found the DEPT 135 sequence to be the most useful. In this experiment, the quaternary carbons are edited out of the spectrum altogether. 

The 13C NMR spectrum of 64, an amide of 63, showed sixty-two carbon signals of which partial assignments, shown in Table 16, were made based upon distortionless enhancement by polarization transfer(DEPT), H-13C correlation experiments and literature data describing 13C NMR analysis of polyene macrolides. 

The imaging of conversion within the fixed bed was achieved by using a distortionless enhancement by polarization transfer (DEPT) spectroscopy pulse sequence integrated into an imaging sequence, as shown in Fig. 44. In theory, a signal enhancement of up to a factor of 4 (/hZ/c 7i is the gyromagnetic ratio of nucleus i) can be achieved with DEPT. In this dual resonance experiment, initial excitation is on the H channel. Consequently, the repetition time for the DEPT experiment is constrained by Tih (< T lc) where Tn is the Ty relaxation time of... 

The distortionless enhancement by polarization transfer (DEPT) sequence 253) for the J-coupled heteronuclear spin system (J is 13C- H coupling, approximately 135 to 170 Hz) is shown in Fig. 48. The pulse sequence is based on a resolvable spin-spin coupling between two nuclei, one of them (lH) being the polarization source for the... 

Furthermore, the allohimachalane (see Section 13.11.9.1) <1999T14623> as well as boletunones A and B, highly functionalized sesquiterpenes from the fruit body of the mushroom Boletus calopus <20040L823>, have been characterized by 2D-NMR (heteronuclear single quantum correlation (HSQC), HMBC, and 111-COSY). The structure of a drimen-ll,12-acetonide, isolated from Maya s herb, was deduced by means of 111 and 13C NMR, distortionless enhancement by polarization transfer (DEPT), COSY, NOESY, HSQC, and HMBC analyses <2005MRC339>. 

Olive oil samples coming from 13 PDO Italian areas of production were analyzed by 13C NMR DEPT (distortionless enhancement by polarization transfer), a particular pulse sequence used to improve the signal-to-noise ratio of13 C spectra (Vlahov et al., 2001). Olive oils were dissolved... 

Vlahov, G., Shaw, A. D., and Kell, D. B. (1999). Use of 13C nuclear magnetic resonance distortionless enhancement by polarization transfer pulse sequence and multivariate analysis to discriminate olive oil cultivars. JAOCS 76,1223-1231. 

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