活泼氢本身化学位移值就是有一个较大的变动范围吧。
5 p/ M4 F4 i; n8 e& r- ^至于积分值,一般要比按化合物的分子式算出来的比例要小。 ( E% c, c5 o4 h9 I( o1 v
原因很多,H交换是一个,积分基线也是一个。前段时间看Simpson的Organic Structure Determination Using 2-D NMR Spectroscopy,里面有提到:
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There are several possible reasons to account for why we observe the low integral values for 1H’s bound to heteroatoms despite having a sufficiently long relaxation delay between scans. First, relaxation (T 2 ) may occur to a greater extent for those 1H’s whose signals are broad as a result of the time delay between the read pulse and the start of the digitization of the FID. Because a broad resonance in the frequency domain corresponds to a rapidly decaying signal amplitude in the time domain, broad resonances will often generate low integrals. A second possible reason for a low integral value is that baseline correction of the spectrum may wipe out the edges of broad resonances, thus subtracting intensity from the peak. A third possible reason for a low integral value of a 1H on a heteroatom may result from partial chemical exchange of these 1H’s with deuterons ( 2H’s) in the solvent, especially if the solvent is deuterated water or methanol
0 J* y& |. z; R[此贴子已经被作者于2009-10-28 19:00:43编辑过]
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