核磁谱图NMR常见溶剂峰杂质峰分析-(中文版).doc

核磁谱图NMR常见溶剂峰杂质峰分析-(中文版).doc

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时间:2020-03-20

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1、测试核磁的样品一般要求比较纯,并且能够溶解在氘代试剂中,这样才能测得高分辨率的图谱。为不干扰谱图,所用溶剂分子中的氢都应被氘取代,但难免有氢的残余(1%左右),这样就会产生溶剂峰;除了残存的质子峰外,溶剂中有时会有微量的H2O而产生水峰,而且这个H2O峰的位置也会因溶剂的不同而不同;另外,在样品(或制备过程)中,也难免会残留一些杂质,在图谱上就会有杂质峰,应注意识别。常用氘代溶剂和杂质峰在1H谱中的化学位移单位:ppm溶剂—CDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3OHD2O溶剂峰—7.262.052.497.161.943.31

2、4.80水峰—1.562.843.330.402.134.87—乙酸—2.101.961.911.551.961.992.08丙酮—2.172.092.091.552.082.152.22乙腈—2.102.052.071.551.962.032.06苯—7.367.367.377.157.377.33—叔丁醇CH31.281.181.111.051.161.401.24OH——4.191.552.18——叔丁基甲醚CCH31.191.131.111.071.141.151.21OCH33.223.133.083.043.133.203.22氯仿—7.26

3、8.028.326.157.587.90—环己烷—1.431.431.401.401.441.45—1,2-二氯甲烷3.733.873.902.903.813.78—二氯甲烷—5.305.635.764.275.445.49—乙醚CH3(t)1.211.111.091.111.121.181.17CH2(q)3.483.413.383.263.423.493.56二甲基甲酰胺CH8.027.967.957.637.927.797.92CH32.962.942.892.362.892.993.01CH32.882.782.731.862.772.862.8

4、5二甲基亚砜—2.622.522.541.682.502.652.71二氧杂环—3.713.593.573.353.603.663.75乙醇CH3(t)1.251.121.060.961.121.191.17CH2(q)3.723.573.443.343.543.603.65OH(s)1.323.393.63—2.47——乙酸乙酯CH3CO2.051.971.991.651.972.012.07OCH2(q)4.124.054.033.894.064.094.14CH3(t)1.261.201.170.921.201.241.24甲乙酮CH3CO2.14

5、2.072.071.582.062.122.19CH2(q)2.462.452.431.812.432.503.18CH3(t)1.060.960.910.850.961.011.26乙二醇—3.763.283.343.413.513.593.65润滑脂CH3(m)0.860.87—0.920.860.88—CH2(br)1.261.29—1.361.271.29—正己烷CH3(t)0.880.880.860.890.890.90—CH2(m)1.261.281.251.241.281.29—甲醇CH33.493.313.163.073.283.343.

6、34OH1.093.124.012.16——正戊烷CH3(t)0.880.880.860.870.890.90—CH2(m)1.271.271.271.231.291.29—异丙醇CH3(d)1.221.101.040.951.091.501.17CH4.043.903.783.673.873.924.02硅脂—0.070.13—0.290.080.10—四氢呋喃CH21.851.791.761.401.801.871.88CH2O3.763.633.603.573.643.713.74甲苯CH32.362.322.302.112.332.32—CH(o

7、/p)7.177.207.187.027.307.16—CH(m)7.257.207.257.137.307.16—三乙基胺CH31.030.960.930.960.961.050.99CH22.532.452.432.402.452.582.57石油醚—0.5-1.50.6-1.9—————

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