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From a 1H-decoupled carbon (13C) spectrum useful information about 13C chemical shifts is obtained. Alternatively, carbon multiplicity and 1H-13C coupling constants can be determined from the gated decoupled methodology and quantitative measurements can be made from the inverse gated methodology.REQUIREMENTS
Easy implementation on AVANCE spectrometerVERSIONS
The basic pulse sequence to record a standard proton spectrum consists of the following steps:EXPERIMENTAL DETAILSAn important aspect to consider is the broadband proton decoupling. It can be applied during the relaxation and/or during the acquisition periods:
- Relaxation period (d1) to achieve a pre-equilibrium state.
- Read pulse (p1) to create transverse magnetization.
- Acquisition during the t2 (acq) period.
- Gated decoupled methodology: Proton decoupling is only applied during the relaxation period. From the resulting 1H-coupled 13C spectrum carbon multiplicities, and direct and long range 1H-13C coupling constants can be determined.
- Inverse gated decoupled methodology: Proton decoupling is only applied during the acquisition period. In this case, no polarization transfer from 1H to 13C via NOE takes place and therefore, the resulting 1H-coupled 13C spectrum can be used for quantitative measurements.
The 13C spectrum is usually acquired, processed and plotted in a fully automated way. Minor changes from a predefined parameter set are required. For routine applications, a 30º-45º pulse with a short relaxation delay (1 second) is usually applied.SPECTRAIn demanding applications, good accuracy is advisable to obtain reliable integration values. In this case, the 13C spectrum is recorded with a 90º pulse and a long relaxation period (5*T1(13C)) is used to avoid partial signal saturation.
For further details on practical implementation on AVANCE spectrometers see:
Recording a 1H-decoupled 13C spectrum 1H-coupled 13C spectrum 1H-decoupled 13C spectrum(without NOE)
The 13C spectrum displays resonance intensities vs frequency. The signals are referenced to the TMS signal (0 ppm) or to the internal deuterated solvent.RELATED TOPICS
See 13C Spectra
Assignment of the 13C spectrum is usually performed by using other NMR methods. As a general strategy:
- Carbon multiplicity is determined from 1D DEPT experiments.
- Correlation with 1H nuclei via 1J(XH) is achieved from HETCOR-type or HMQC-type experiments.
- Correlation with 1H nuclei via nJ(CH) is achieved from HMBC-type experiments.