核磁共振定量NMR 实验
实验考虑：
Good signal to noise 好的信燥比
90° pulse sufficiently short to excite the entire region uniformly
Delay between pulses of at least 5 T1’s 脉冲延迟至少T1的5倍
Flat base line to start with and baseline correction 基线平坦和基线校正
Filter bandwidth set to at least twice the sw
Enough data points to give 15 to 20 points per peak - remember that you lose half the points to the imaginaries in Fourier transformation
Acquire at least 32k and zero fill several times – memory is cheap
Exception to 32k for other nuclei requiring 1H decoupling - it is important to limit the acquisition time to as short as possible to avoid NOE build up during the acquisition so < 32k may be necessary with zero filling to make up the difference
Zero filling should only be done after dc correction and line broadening otherwise it introduces baseline artifacts
Gated decoupling for non-hydrogen analysis
Careful phasing on a spectrum that has been greatly expanded in the vertical direction
Careful integration
Place a single integral over the spectral limits of interest
Adjust bias and slope on the full integral
Cut integral into smaller regions as close as possible to the peak
Consistently include or exclude satellites or account for them when they overlap
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