核磁常见溶剂峰
核磁谱图NMR常见溶剂峰杂质峰分析中文版
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)2SO? C6D6?? ?CD3CN?? CD3OH?? D2O溶剂峰—7.26 2.05 2.49 7.16 1.94 3.31 4.80水峰— 1.56 2.84 3.33 0.40 2.13 4.87 —乙酸— 2.10 1.96 1.91 1.55 1.96 1.99 2.08丙酮— 2.17 2.09 2.09 1.55 2.08 2.15 2.22乙腈— 2.10 2.05 2.07 1.55 1.96 2.03 2.06苯—7.36 7.36 7.37 7.15 7.37 7.33 —叔丁醇CH3 1.28 1.18 1.11 1.05 1.16 1.40 1.24OH —— 4.19 1.55 2.18 ——叔丁基甲醚CCH3 1.19 1.13 1.11 1.07 1.14 1.15 1.21OCH3 3.22 3.13 3.08 3.04 3.13 3.20 3.22氯仿—7.26 8.02 8.32 6.15 7.58 7.90 —环己烷— 1.43 1.43 1.40 1.40 1.44 1.45 —1,2-二氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78 —二氯甲烷— 5.30 5.63 5.76 4.27 5.44 5.49 —乙醚 CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17CH2(q) 3.48 3.41 3.38 3.26 3.42 3.49 3.56二甲基甲酰胺CH 8.02 7.96 7.95 7.63 7.92 7.79 7.92CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3 2.88 2.78 2.73 1.86 2.77 2.86 2.85二甲基亚砜— 2.62 2.52 2.54 1.68 2.50 2.65 2.71二氧杂环— 3.71 3.59 3.57 3.35 3.60 3.66 3.75 乙醇 CH3(t) 1.25 1.12 1.06 0.96 1.12 1.19 1.17 CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH(s) 1.32 3.39 3.63 — 2.47 ——乙酸乙酯CH3CO 2.05 1.97 1.99 1.65 1.97 2.01 2.07 OCH2(q) 4.12 4.05 4.03 3.89 4.06 4.09 4.14CH3(t) 1.26 1.20 1.17 0.92 1.20 1.24 1.24甲乙酮CH3CO 2.14 2.07 2.07 1.58 2.06 2.12 2.19 CH2(q) 2.46 2.45 2.43 1.81 2.43 2.50 3.18CH3(t) 1.06 0.96 0.91 0.85 0.96 1.01 1.26乙二醇— 3.76 3.28 3.34 3.41 3.51 3.59 3.65润滑脂 CH3(m) 0.86 0.87 —0.92 0.86 0.88 —CH2(br) 1.26 1.29 — 1.36 1.27 1.29 —正己烷CH3(t) 0.88 0.88 0.86 0.89 0.89 0.90 —CH2 (m) 1.26 1.28 1.25 1.24 1.28 1.29 —甲醇CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH 1.09 3.12 4.01 2.16 ——正戊烷 CH3(t) 0.88 0.88 0.86 0.87 0.89 0.90 —CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29 —异丙醇CH3(d) 1.22 1.10 1.04 0.95 1.09 1.50 1.17 CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02 硅脂—0.07 0.13 —0.29 0.08 0.10 —四氢呋喃 CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O 3.76 3.63 3.60 3.57 3.64 3.71 3.74 甲苯 CH3 2.36 2.32 2.30 2.11 2.33 2.32 —CH（o/p）7.17 7.20 7.18 7.02 7.30 7.16 —CH（m） 7.25 7.20 7.25 7.13 7.30 7.16 —三乙基胺 CH3 1.03 0.96 0.93 0.96 0.96 1.05 0.99 CH2 2.53 2.45 2.43 2.40 2.45 2.58 2.57 石油醚—0.5-1.5 0.6-1.9 —————。
NMR常见溶剂峰和水峰
注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。
对于酚羟基能够出峰。
芳香化合物还是芳香甙，都为首选。
吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。
极性大的化合物可采用氘代丙酮、重水等。
针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。
丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙5；1小极性石：丙2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1 含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶剂: CD3COCD3, C6D6, CD3CN。
极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。
CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。
Solvent化学位移(ppm)水峰位移(ppm)CDCl37.26 1.56DMSO 2.50 3.33CD3OD 3.31 4.87D2O 4.79CD3COCD3 2.05 2.84Welcome To Download !!!欢迎您的下载，资料仅供参考！。
核磁谱图NMR常见溶剂峰杂质峰分析_(中文版)之欧阳育创编
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)2SO C6D6 CD3CN CD3OH D2O溶剂峰—7.26 2.05 2.49 7.16 1.94 3.31 4.80水峰—1.562.843.33 0.40 2.134.87 —乙酸—2.10 1.96 1.91 1.55 1.96 1.99 2.08丙酮—2.17 2.09 2.09 1.55 2.08 2.15 2.22乙腈—2.10 2.05 2.07 1.55 1.96 2.03 2.06苯—7.36 7.36 7.37 7.15 7.37 7.33 —叔丁醇CH3 1.28 1.18 1.11 1.05 1.16 1.40 1. 24OH —— 4.19 1.55 2.18 ——叔丁基甲醚CCH3 1.19 1.13 1.11 1.07 1.14 1.15 1.21OCH3 3.22 3.13 3.08 3.04 3.13 3.2 0 3.22氯仿—7.26 8.02 8.32 6.15 7.58 7.90 —环己烷—1.43 1.43 1.40 1.40 1.44 1.45 —1,2-二氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78 —二氯甲烷—5.30 5.63 5.76 4.27 5.44 5.49 —乙醚 CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17CH2(q) 3.48 3.41 3.38 3.26 3.42 3.4 9 3.56二甲基甲酰胺CH 8.02 7.96 7.95 7.63 7.92 7.79 7.92CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.0186 2.85二甲基亚砜—2.62 2.52 2.54 1.68 2.50 2.65 2.71二氧杂环—3.71 3.59 3.57 3.35 3.60 3.66 3.75乙醇 CH3(t) 1.25 1.12 1.06 0.96 1.12 1.19 1.17CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH(s) 1.32 3.39 3.63 —2.47 ——乙酸乙酯CH3CO2.05 1.97 1.99 1.65 1.97 2.01 2.07OCH2(q) 4.12 4.05 4.03 3.89 4.06 4 .09 4.14CH3(t) 1.26 1.20 1.17 0.92 1.20 1.24 1.24甲乙酮CH3CO 2.14 2.07 2.07 1.58 2.06 2.12 2.1950 3.18CH3(t) 1.06 0.96 0.91 0.85 0.96 1.01 1.26乙二醇—3.76 3.28 3.34 3.41 3.51 3.59 3.6 5润滑脂 CH3(m) 0.86 0.87 —0.92 0.86 0.88 —CH2(br) 1.26 1.29 —1.36 1.27 1.29 —正己烷CH3(t) 0.88 0.88 0.86 0.89 0.89 0.90 —CH2(m) 1.26 1.28 1.25 1.24 1.28 1.29 —甲醇 CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34OH 1.09 3.12 4.01 2.16 ——正戊烷 CH3(t) 0.88 0.88 0.86 0.87 0.89 0.90 —CH2(m) 1.27 1.27 1.27 1.23 1.29 1 .29 —异丙醇CH3(d) 1.22 1.10 1.04 0.95 1.09 1.50 1.17CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02硅脂— 0.07 0.13 —0.29 0.08 0.10 —四氢呋喃 CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88CH2O 3.76 3.63 3.60 3.57 3.64 3.7 1 3.74甲苯 CH3 2.36 2.32 2.30 2.11 2.33 2.3 2 —CH（o/p）7.17 7.20 7.18 7.02 7.30 7.16 —CH（m） 7.25 7.20 7.25 7.13 7.30 7.16 —三乙基胺 CH3 1.03 0.96 0.93 0.96 0.96 1.05 0.99CH2 2.53 2.45 2.43 2.40 2.45 2.58 2.57石油醚— 0.5-1.5 0.6-1.9 —————。
NMR常见溶剂峰和水峰
注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。
对于酚羟基能够出峰。
芳香化合物还是芳香甙，都为首选。
吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。
极性大的化合物可采用氘代丙酮、重水等。
针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。
丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙 5；1小极性石：丙 2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1 含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶剂: CD3COCD3, C6D6, CD3CN。
极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。
CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。
Solvent 化学位移(ppm) 水峰位移(ppm)CDCl3 7.26 1.56DMSO 2.50 3.33CD3OD 3.31 4.87D2O 4.79CD3COCD3 2.05 2.84。
NMR常见溶剂峰和水峰
注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。
对于酚羟基能够出峰。
芳香化合物还是芳香甙，都为首选。
吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。
极性大的化合物可采用氘代丙酮、重水等。
针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。
丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙 5；1小极性石：丙 2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1 含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶剂: CD3COCD3, C6D6, CD3CN。
极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。
CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。
Solvent 化学位移(ppm) 水峰位移(ppm)CDCl3 7.26 1.56DMSO 2.50 3.33CD3OD 3.31 4.87D2O 4.79CD3COCD3 2.05 2.84。
核磁谱图NMR常见溶剂峰杂质峰分析_(中文版)
之樊仲川亿创作测试核磁的样品一般要求比较纯，而且能够溶解在氘代试剂中，这样才干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，但难免有氢的残存（1%左右），这样就会发生溶剂峰；除了残存的质子峰外，溶剂中有时会有微量的H2O而发生水峰，而且这个H2O峰的位置也会因溶剂的分歧而分歧；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。
经常使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)2SO C6D6 CD3CN CD3 OH D2O水峰—1.562.843.33 0 .40 2.134.87 —苯—7.36 7.36 7.377.15 7.37 7.33 —OH ——4.19 1.55 2.18——叔丁基甲醚氯仿—7.26 8.02 8.326.157.58 7.90 —环己烷—1.43 1.43 1.401.40 1.44 1.45 —1,2-二氯甲烷 3.73 3.87 3.902.903.81 3.78 —二氯甲烷—5.30 5.63 5.764.275.44 5.49 —二甲基甲酰胺OH(s) 1.32 3.393.63 —2.47 ——润滑脂CH3(m) 0.86 0.87 —0.92 0.86 0.88—CH2(br) 1.26 1.29—1.36 1.27 1.29—正己烷CH3(t) 0.88 0.88 0.860.89 0.89 0.90—CH2(m) 1.26 1.28 1.251.24 1.28 1.29 —OH 1.09 3.124.01 2.16 ——正戊烷CH3(t) 0.88 0.88 0.860.87 0.89 0.90—CH2(m) 1.27 1.271.27 1.23 1.29 1.29—硅脂—0.07 0.13 —0.29 0.08 0.10—甲苯CH3 2.36 2.32 2 .30 2.11 2.33 2.32 —CH（o/p）7.17 7.20 7.18 7.027.30 7.16 —CH（m）7.25 7.20 7.25 7.13 7.30 7.16 —石油醚— 0.5-1.5 0.6-1.9 —————。
NMR常见溶剂峰和水峰
注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。
对于酚羟基能够出峰。
芳香化合物还是芳香甙，都为首选。
吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。
极性大的化合物可采用氘代丙酮、重水等。
针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。
丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙 5；1小极性石：丙 2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1 含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶剂: CD3COCD3, C6D6, CD3CN。
极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。
CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。
Solvent 化学位移(ppm) 水峰位移(ppm)CDCl3 7.26 1.56DMSO 2.50 3.33CD3OD 3.31 4.87D2O 4.79CD3COCD3 2.05 2.84。
NMR常见溶剂峰和水峰
注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。
对于酚羟基能够出峰。
芳香化合物还是芳香甙，都为首选。
吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。
极性大的化合物可采用氘代丙酮、重水等。
针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。
丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙 5；1小极性石：丙 2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1 含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶剂: CD3COCD3, C6D6, CD3CN。
极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。
CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。
Solvent 化学位移(ppm) 水峰位移(ppm)CDCl3 7.26 1.56DMSO 2.50 3.33CD3OD 3.31 4.87D2O 4.79CD3COCD3 2.05 2.84。
核磁谱图nmr常见溶剂峰杂质峰分析中文版
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)2SO C6D6 CD3CN CD3OH D2O溶剂峰—7.26 2.05 2.49 7.16 1.94 3.31 4.80水峰— 1.56 2.84 3.33 0.40 2.13 4.87 —乙酸— 2.10 1.96 1.91 1.55 1.96 1.99 2.08丙酮— 2.17 2.09 2.09 1.55 2.08 2.15 2.22乙腈— 2.10 2.05 2.07 1.55 1.96 2.03 2.06苯—7.36 7.36 7.37 7.15 7.37 7.33 —叔丁醇CH3 1.28 1.18 1.11 1.05 1.16 1.40 1.24OH —— 4.19 1.55 2.18 ——叔丁基甲醚CCH3 1.19 1.13 1.11 1.07 1.14 1.15 1.21OCH3 3.22 3.13 3.08 3.04 3.13 3.20 3.22氯仿—7.26 8.02 8.32 6.15 7.58 7.90 —环己烷— 1.43 1.43 1.40 1.40 1.44 1.45 —1,2-二氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78 —二氯甲烷— 5.30 5.63 5.76 4.27 5.44 5.49 —乙醚 CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17CH2(q) 3.48 3.41 3.38 3.26 3.42 3.49 3.56二甲基甲酰胺CH 8.02 7.96 7.95 7.63 7.92 7.79 7.92CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3 2.88 2.78 2.73 1.86 2.77 2.86 2.85二甲基亚砜— 2.62 2.52 2.54 1.68 2.50 2.65 2.71二氧杂环— 3.71 3.59 3.57 3.35 3.60 3.66 3.75乙醇 CH3(t) 1.25 1.12 1.06 0.96 1.12 1.19 1.17CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH(s) 1.32 3.39 3.63 — 2.47 ——乙酸乙酯CH3CO 2.05 1.97 1.99 1.65 1.97 2.01 2.07 OCH2(q) 4.12 4.05 4.03 3.89 4.06 4.09 4.14CH3(t) 1.26 1.20 1.17 0.92 1.20 1.24 1.24甲乙酮CH3CO 2.14 2.07 2.07 1.58 2.06 2.12 2.19 CH2(q) 2.46 2.45 2.43 1.81 2.43 2.50 3.18CH3(t) 1.06 0.96 0.91 0.85 0.96 1.01 1.26乙二醇— 3.76 3.28 3.34 3.41 3.51 3.59 3.65润滑脂 CH3(m) 0.86 0.87 —0.92 0.86 0.88 —CH2(br) 1.26 1.29 — 1.36 1.27 1.29 —正己烷CH3(t) 0.88 0.88 0.86 0.89 0.89 0.90 —CH2 (m) 1.26 1.28 1.25 1.24 1.28 1.29 —甲醇CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH 1.09 3.12 4.01 2.16 ——正戊烷 CH3(t) 0.88 0.88 0.86 0.87 0.89 0.90 —CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29 —异丙醇CH3(d) 1.22 1.10 1.04 0.95 1.09 1.50 1.17 CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02 硅脂—0.07 0.13 —0.29 0.08 0.10 —四氢呋喃 CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O 3.76 3.63 3.60 3.57 3.64 3.71 3.74 甲苯 CH3 2.36 2.32 2.30 2.11 2.33 2.32 —CH（o/p）7.17 7.20 7.18 7.02 7.30 7.16 —CH（m） 7.25 7.20 7.25 7.13 7.30 7.16 —三乙基胺 CH3 1.03 0.96 0.93 0.96 0.96 1.05 0.99 CH2 2.53 2.45 2.43 2.40 2.45 2.58 2.57 石油醚—0.5-1.5 0.6-1.9 —————。
核磁谱图NMR常见溶剂峰杂质峰分析_(中文版)
之阳早格格创做尝试核磁的样品普遍央供比较杂，而且不妨溶解正在氘代试剂中，那样才搞测得下辨别率的图谱.为没有搞扰谱图，所用溶剂分子中的氢皆应被氘与代，但是易免有氢的残存（1%安排），那样便会爆收溶剂峰；除了残存的量子峰中，溶剂中偶尔会有微量的H2O而爆收火峰，而且那个H2O峰的位子也会果溶剂的分歧而分歧；其余，正在样品（或者造备历程）中，也易免会残留一些杂量，正在图谱上便会有杂量峰，应注意辨别.时常使用氘代溶剂战杂量峰正在1H谱中的化教位移单位：ppm溶剂—CDCl3 (CD3)2CO (CD3)2SO C6D6 CD3CN CD3OH D2 O火峰—1.562.843.33 0.40 2.134.87 —苯—7.36 7.36 7.37 7.15 7.37 7.33 —OH —— 4.19 1.55 2.18 ——叔丁基甲醚氯仿—7.26 8.02 8.32 6.15 7.58 7.90 —环己烷—1.43 1.43 1.40 1.40 1.44 1.45 —1,2-两氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78 —两氯甲烷—5.30 5.63 5.76 4.27 5.44 5.49 —两甲基甲酰胺OH(s) 1.32 3.39 3.63 —2.47 ——润滑脂 CH3(m) 0.86 0.87 —0.92 0.86 0.88 —CH2(br) 1.26 1.29 —1.36 1.27 1.29 —正己烷CH3(t) 0.88 0.88 0.86 0.89 0.89 0.90 —CH2(m) 1.26 1.28 1.25 1.24 1.28 1.29 —OH 1.09 3.12 4.01 2.16 ——正戊烷 CH3(t) 0.88 0.88 0.86 0.87 0.89 0.90 —CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29 —硅脂— 0.07 0.13 —0.29 0.08 0.10 —甲苯 CH3 2.36 2.32 2.30 2.11 2.33 2.3 2 —CH（o/p）7.17 7.20 7.18 7.02 7.30 7.16 —CH（m） 7.25 7.20 7.25 7.13 7.30 7.16 —石油醚— 0.5-1.5 0.6-1.9 —————。
核磁溶剂峰和杂质峰
常用氘代溶剂和杂质峰在1H-NMR谱中的化学位移如下表所示（单位：ppm）溶剂—CDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OH D2O溶剂峰—7.26 2.05 2.497.16 1.94 3.31 4.80水峰— 1.56 2.84 3.330.40 2.13 4.87—乙酸— 2.10 1.96 1.91 1.55 1.96 1.99 2.08丙酮— 2.17 2.09 2.09 1.55 2.08 2.15 2.22乙腈— 2.10 2.05 2.07 1.55 1.96 2.03 2.06苯—7.367.367.377.157.377.33—叔丁醇CH3 1.28 1.18 1.11 1.05 1.16 1.40 1.24 OH—— 4.19 1.55 2.18——乙醇CH3(t) 1.25 1.12 1.060.96 1.12 1.19 1.17 CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH(s) 1.32 3.39 3.63— 2.47——乙酸乙酯CH3CO 2.05 1.97 1.99 1.65 1.97 2.01 2.07 OCH2(q) 4.12 4.05 4.03 3.89 4.06 4.09 4.14CH3(t) 1.26 1.20 1.170.92 1.20 1.24 1.24乙二醇— 3.76 3.28 3.34 3.41 3.51 3.59 3.65正己烷CH3(t)0.880.880.860.890.890.90—CH2(m) 1.26 1.28 1.25 1.24 1.28 1.29—甲醇CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH 1.09 3.12 4.01 2.16——正戊烷CH3(t)0.880.880.860.870.890.90—CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29—异丙醇CH3(d) 1.22 1.10 1.040.95 1.09 1.50 1.17 CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02四氢呋喃CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O 3.76 3.63 3.60 3.57 3.64 3.71 3.74甲苯CH3 2.36 2.32 2.30 2.11 2.33 2.32—CH(o/p)7.177.207.187.027.307.16—CH（m）7.257.207.257.137.307.16—氯仿—7.268.028.32 6.157.587.90—环己烷— 1.43 1.43 1.40 1.40 1.44 1.45—1,2-二氯甲烷— 3.73 3.87 3.90 2.90 3.81 3.78—二氯甲烷— 5.30 5.63 5.76 4.27 5.44 5.49—乙醚CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17 CH2(q) 3.48 3.41 3.38 3.26 3.42 3.49 3.56二甲基甲酰胺CH8.027.967.957.637.927.797.92 CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3 2.88 2.78 2.73 1.86 2.77 2.86 2.85二甲基亚砜— 2.62 2.52 2.54 1.68 2.50 2.65 2.71二氧杂环— 3.71 3.59 3.57 3.35 3.60 3.66 3.75测试核磁时，所用溶剂分子中的氢都应被氘取代，但难免有残余，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。
核磁溶剂峰列表
NMR Chemical Shifts of Common Laboratory Solvents as Trace Impurities Hugo E.Gottlieb,*Vadim Kotlyar,andAbraham Nudelman*Department of Chemistry,Bar-Ilan University,Ramat-Gan52900,IsraelReceived June27,1997In the course of the routine use of NMR as an aid for organic chemistry,a day-to-day problem is the identifica-tion of signals deriving from common contaminants (water,solvents,stabilizers,oils)in less-than-analyti-cally-pure samples.This data may be available in the literature,but the time involved in searching for it may be considerable.Another issue is the concentration dependence of chemical shifts(especially1H);results obtained two or three decades ago usually refer to much more concentrated samples,and run at lower magnetic fields,than today’s practice.We therefore decided to collect1H and13C chemical shifts of what are,in our experience,the most popular “extra peaks”in a variety of commonly used NMR solvents,in the hope that this will be of assistance to the practicing chemist.Experimental SectionNMR spectra were taken in a Bruker DPX-300instrument (300.1and75.5MHz for1H and13C,respectively).Unless otherwise indicated,all were run at room temperature(24(1°C).For the experiments in the last section of this paper,probe temperatures were measured with a calibrated Eurotherm840/T digital thermometer,connected to a thermocouple which was introduced into an NMR tube filled with mineral oil to ap-proximately the same level as a typical sample.At each temperature,the D2O samples were left to equilibrate for at least 10min before the data were collected.In order to avoid having to obtain hundreds of spectra,we prepared seven stock solutions containing approximately equal amounts of several of our entries,chosen in such a way as to prevent intermolecular interactions and possible ambiguities in assignment.Solution1:acetone,tert-butyl methyl ether,di-methylformamide,ethanol,toluene.Solution2:benzene,di-methyl sulfoxide,ethyl acetate,methanol.Solution3:acetic acid,chloroform,diethyl ether,2-propanol,tetrahydrofuran. Solution4:acetonitrile,dichloromethane,dioxane,n-hexane, HMPA.Solution5:1,2-dichloroethane,ethyl methyl ketone, n-pentane,pyridine.Solution6:tert-butyl alcohol,BHT,cyclo-hexane,1,2-dimethoxyethane,nitromethane,silicone grease, triethylamine.Solution7:diglyme,dimethylacetamide,ethyl-ene glycol,“grease”(engine oil).For D2O.Solution1:acetone, tert-butyl methyl ether,dimethylformamide,ethanol,2-propanol. Solution2:dimethyl sulfoxide,ethyl acetate,ethylene glycol, methanol.Solution3:acetonitrile,diglyme,dioxane,HMPA, pyridine.Solution4:1,2-dimethoxyethane,dimethylacetamide, ethyl methyl ketone,triethylamine.Solution5:acetic acid,tert-butyl alcohol,diethyl ether,tetrahydrofuran.In D2O and CD3OD nitromethane was run separately,as the protons exchanged with deuterium in presence of triethylamine.ResultsProton Spectra(Table1).A sample of0.6mL of the solvent,containing1µL of TMS,1was first run on its own.From this spectrum we determined the chemical shifts of the solvent residual peak2and the water peak. It should be noted that the latter is quite temperature-dependent(vide infra).Also,any potential hydrogen-bond acceptor will tend to shift the water signal down-field;this is particularly true for nonpolar solvents.In contrast,in e.g.DMSO the water is already strongly hydrogen-bonded to the solvent,and solutes have only a negligible effect on its chemical shift.This is also true for D2O;the chemical shift of the residual HDO is very temperature-dependent(vide infra)but,maybe counter-intuitively,remarkably solute(and pH)independent. We then added3µL of one of our stock solutions to the NMR tube.The chemical shifts were read and are presented in Table 1.Except where indicated,the coupling constants,and therefore the peak shapes,are essentially solvent-independent and are presented only once.For D2O as a solvent,the accepted reference peak(δ)0)is the methyl signal of the sodium salt of3-(trimeth-ylsilyl)propanesulfonic acid;one crystal of this was added to each NMR tube.This material has several disadvan-tages,however:it is not volatile,so it cannot be readily eliminated if the sample has to be recovered.In addition, unless one purchases it in the relatively expensive deuterated form,it adds three more signals to the spectrum(methylenes1,2,and3appear at2.91,1.76, and0.63ppm,respectively).We suggest that the re-sidual HDO peak be used as a secondary reference;we find that if the effects of temperature are taken into account(vide infra),this is very reproducible.For D2O, we used a different set of stock solutions,since many of the less polar substrates are not significantly water-soluble(see Table1).We also ran sodium acetate and sodium formate(chemical shifts: 1.90and8.44ppm, respectively).Carbon Spectra(Table2).To each tube,50µL of the stock solution and3µL of TMS1were added.The solvent chemical shifts3were obtained from the spectra containing the solutes,and the ranges of chemical shifts(1)For recommendations on the publication of NMR data,see: IUPAC Commission on Molecular Structure and Spectroscopy.Pure Appl.Chem.1972,29,627;1976,45,217.(2)I.e.,the signal of the proton for the isotopomer with one less deuterium than the perdeuterated material,e.g.,C H Cl3in CDCl3or C6D5H in C6D6.Except for CHCl3,the splitting due to J HD is typically observed(to a good approximation,it is1/6.5of the value of the corresponding J HH).For CHD2groups(deuterated acetone,DMSO, acetonitrile),this signal is a1:2:3:2:1quintet with a splitting of ca.2 Hz.(3)In contrast to what was said in note2,in the13C spectra the solvent signal is due to the perdeuterated isotopomer,and the one-bond couplings to deuterium are always observable(ca.20-30Hz). Figure1.Chemical shift of H DO as a function of tempera-ture..Chem.1997,62,7512-7515S0022-3263(97)01176-6CCC:$14.00©1997American Chemical Societyshow their degree of variability.Occasionally,in order to distinguish between peaks whose assignment was ambiguous,a further1-2µL of a specific substrate were added and the spectra run again.Table1.1H NMR Dataproton mult CDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent residual peak7.26 2.05 2.507.16 1.94 3.31 4.79 H2O s 1.56 2.84a 3.33a0.40 2.13 4.87acetic acid CH3s 2.10 1.96 1.91 1.55 1.96 1.99 2.08 acetone CH3s 2.17 2.09 2.09 1.55 2.08 2.15 2.22 acetonitrile CH3s 2.10 2.05 2.07 1.55 1.96 2.03 2.06 benzene CH s7.367.367.377.157.377.33tert-butyl alcohol CH3s 1.28 1.18 1.11 1.05 1.16 1.40 1.24 OH c s 4.19 1.55 2.18tert-butyl methyl ether CCH3s 1.19 1.13 1.11 1.07 1.14 1.15 1.21 OCH3s 3.22 3.13 3.08 3.04 3.13 3.20 3.22 BHT b ArH s 6.98 6.96 6.877.05 6.97 6.92OH c s 5.01 6.65 4.79 5.20ArCH3s 2.27 2.22 2.18 2.24 2.22 2.21ArC(CH3)3s 1.43 1.41 1.36 1.38 1.39 1.40chloroform CH s7.268.028.32 6.157.587.90 cyclohexane CH2s 1.43 1.43 1.40 1.40 1.44 1.451,2-dichloroethane CH2s 3.73 3.87 3.90 2.90 3.81 3.78 dichloromethane CH2s 5.30 5.63 5.76 4.27 5.44 5.49diethyl ether CH3t,7 1.21 1.11 1.09 1.11 1.12 1.18 1.17 CH2q,7 3.48 3.41 3.38 3.26 3.42 3.49 3.56 diglyme CH2m 3.65 3.56 3.51 3.46 3.53 3.61 3.67 CH2m 3.57 3.47 3.38 3.34 3.45 3.58 3.61OCH3s 3.39 3.28 3.24 3.11 3.29 3.35 3.37 1,2-dimethoxyethane CH3s 3.40 3.28 3.24 3.12 3.28 3.35 3.37 CH2s 3.55 3.46 3.43 3.33 3.45 3.52 3.60 dimethylacetamide CH3CO s 2.09 1.97 1.96 1.60 1.97 2.07 2.08 NCH3s 3.02 3.00 2.94 2.57 2.96 3.31 3.06NCH3s 2.94 2.83 2.78 2.05 2.83 2.92 2.90 dimethylformamide CH s8.027.967.957.637.927.977.92 CH3s 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3s 2.88 2.78 2.73 1.86 2.77 2.86 2.85 dimethyl sulfoxide CH3s 2.62 2.52 2.54 1.68 2.50 2.65 2.71 dioxane CH2s 3.71 3.59 3.57 3.35 3.60 3.66 3.75 ethanol CH3t,7 1.25 1.12 1.060.96 1.12 1.19 1.17 CH2q,7d 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH s c,d 1.32 3.39 4.63 2.47ethyl acetate CH3CO s 2.05 1.97 1.99 1.65 1.97 2.01 2.07C H2CH3q,7 4.12 4.05 4.03 3.89 4.06 4.09 4.14CH2C H3t,7 1.26 1.20 1.170.92 1.20 1.24 1.24 ethyl methyl ketone CH3CO s 2.14 2.07 2.07 1.58 2.06 2.12 2.19C H2CH3q,7 2.46 2.45 2.43 1.81 2.43 2.50 3.18CH2C H3t,7 1.060.960.910.850.96 1.01 1.26 ethylene glycol CH s e 3.76 3.28 3.34 3.41 3.51 3.59 3.65“grease”f CH3m0.860.870.920.860.88CH2br s 1.26 1.29 1.36 1.27 1.29n-hexane CH3t0.880.880.860.890.890.90CH2m 1.26 1.28 1.25 1.24 1.28 1.29HMPA g CH3d,9.5 2.65 2.59 2.53 2.40 2.57 2.64 2.61 methanol CH3s h 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH s c,h 1.09 3.12 4.01 2.16nitromethane CH3s 4.33 4.43 4.42 2.94 4.31 4.34 4.40 n-pentane CH3t,70.880.880.860.870.890.90CH2m 1.27 1.27 1.27 1.23 1.29 1.292-propanol CH3d,6 1.22 1.10 1.040.95 1.09 1.50 1.17 CH sep,6 4.04 3.90 3.78 3.67 3.87 3.92 4.02 pyridine CH(2)m8.628.588.588.538.578.538.52 CH(3)m7.297.357.39 6.667.337.447.45CH(4)m7.687.767.79 6.987.737.857.87 silicone grease i CH3s0.070.130.290.080.10 tetrahydrofuran CH2m 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O m 3.76 3.63 3.60 3.57 3.64 3.71 3.74 toluene CH3s 2.36 2.32 2.30 2.11 2.33 2.32CH(o/p)m7.177.1-7.27.187.027.1-7.37.16CH(m)m7.257.1-7.27.257.137.1-7.37.16 triethylamine CH3t,7 1.030.960.930.960.96 1.050.99 CH2q,7 2.53 2.45 2.43 2.40 2.45 2.58 2.57a In these solvents the intermolecular rate of exchange is slow enough that a peak due to HDO is usually also observed;it appears at2.81and3.30ppm in acetone and DMSO,respectively.In the former solvent,it is often seen as a1:1:1triplet,with2J H,D)1Hz. b2,6-Dimethyl-4-tert-butylphenol.c The signals from exchangeable protons were not always identified.d In some cases(see note a),the coupling interaction between the CH2and the OH protons may be observed(J)5Hz).e In CD3CN,the OH proton was seen as a multiplet atδ2.69,and extra coupling was also apparent on the methylene peak.f Long-chain,linear aliphatic hydrocarbons.Their solubility in DMSO was too low to give visible peaks.g Hexamethylphosphoramide.h In some cases(see notes a,d),the coupling interaction between the CH3and the OH protons may be observed(J)5.5Hz).i Poly(dimethylsiloxane).Its solubility in DMSO was too low to give visible peaks.Notes .Chem.,Vol.62,No.21,19977513.Chem.,Vol.62,No.21,1997NotesTable2.13C NMR Data aCDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent signals77.16(0.0629.84(0.0139.52(0.06128.06(0.02 1.32(0.0249.00(0.01206.26(0.13118.26(0.02acetic acid CO175.99172.31171.93175.82173.21175.11177.21 CH320.8120.5120.9520.3720.7320.5621.03 acetone CO207.07205.87206.31204.43207.43209.67215.94 CH330.9230.6030.5630.1430.9130.6730.89 acetonitrile CN116.43117.60117.91116.02118.26118.06119.68 CH3 1.89 1.12 1.030.20 1.790.85 1.47 benzene CH128.37129.15128.30128.62129.32129.34tert-butyl alcohol C69.1568.1366.8868.1968.7469.4070.36 CH331.2530.7230.3830.4730.6830.9130.29 tert-butyl methyl ether OCH349.4549.3548.7049.1949.5249.6649.37 C72.8772.8172.0472.4073.1774.3275.62C C H326.9927.2426.7927.0927.2827.2226.60 BHT C(1)151.55152.51151.47152.05152.42152.85C(2)135.87138.19139.12136.08138.13139.09CH(3)125.55129.05127.97128.52129.61129.49C(4)128.27126.03124.85125.83126.38126.11CH3Ar21.2021.3120.9721.4021.2321.38C H3C30.3331.6131.2531.3431.5031.15C34.2535.0034.3334.3535.0535.36chloroform CH77.3679.1979.1677.7979.1779.44cyclohexane CH226.9427.5126.3327.2327.6327.961,2-dichloroethane CH243.5045.2545.0243.5945.5445.11 dichloromethane CH253.5254.9554.8453.4655.3254.78diethyl ether CH315.2015.7815.1215.4615.6315.4614.77 CH265.9166.1262.0565.9466.3266.8866.42 diglyme CH359.0158.7757.9858.6658.9059.0658.67 CH270.5171.0369.5470.8770.9971.3370.05CH271.9072.6371.2572.3572.6372.9271.63 1,2-dimethoxyethane CH359.0858.4558.0158.6858.8959.0658.67 CH271.8472.4717.0772.2172.4772.7271.49 dimethylacetamide CH321.5321.5121.2921.1621.7621.3221.09 CO171.07170.61169.54169.95171.31173.32174.57NCH335.2834.8937.3834.6735.1735.5035.03NCH338.1337.9234.4237.0338.2638.4338.76 dimethylformamide CH162.62162.79162.29162.13163.31164.73165.53 CH336.5036.1535.7335.2536.5736.8937.54CH331.4531.0330.7330.7231.3231.6132.03 dimethyl sulfoxide CH340.7641.2340.4540.0341.3140.4539.39 dioxane CH267.1467.6066.3667.1667.7268.1167.19 ethanol CH318.4118.8918.5118.7218.8018.4017.47 CH258.2857.7256.0757.8657.9658.2658.05 ethyl acetate C H3CO21.0420.8320.6820.5621.1620.8821.15 CO171.36170.96170.31170.44171.68172.89175.26CH260.4960.5659.7460.2160.9861.5062.32CH314.1914.5014.4014.1914.5414.4913.92 ethyl methyl ketone C H3CO29.4929.3029.2628.5629.6029.3929.49 CO209.56208.30208.72206.55209.88212.16218.43C H2CH336.8936.7535.8336.3637.0937.3437.27CH2C H37.868.037.617.918.148.097.87 ethylene glycol CH263.7964.2662.7664.3464.2264.3063.17“grease”CH229.7630.7329.2030.2130.8631.29n-hexane CH314.1414.3413.8814.3214.4314.45CH2(2)22.7023.2822.0523.0423.4023.68CH2(3)31.6432.3030.9531.9632.3632.73HMPA b CH336.8737.0436.4236.8837.1037.0036.46 methanol CH350.4149.7748.5949.9749.9049.8649.50c nitromethane CH362.5063.2163.2861.1663.6663.0863.22 n-pentane CH314.0814.2913.2814.2514.3714.39CH2(2)22.3822.9821.7022.7223.0823.38CH2(3)34.1634.8333.4834.4534.8935.302-propanol CH325.1425.6725.4325.1825.5525.2724.38 CH64.5063.8564.9264.2364.3064.7164.88 pyridine CH(2)149.90150.67149.58150.27150.76150.07149.18 CH(3)123.75124.57123.84123.58127.76125.53125.12CH(4)135.96136.56136.05135.28136.89138.35138.27 silicone grease CH3 1.04 1.40 1.38 2.10 tetrahydrofuran CH225.6226.1525.1425.7226.2726.4825.67 CH2O67.9768.0767.0367.8068.3368.8368.68 toluene CH321.4621.4620.9921.1021.5021.50C(i)137.89138.48137.35137.91138.90138.85CH(o)129.07129.76128.88129.33129.94129.91CH(m)128.26129.03128.18128.56129.23129.20CH(p)125.33126.12125.29125.68126.28126.29triethylamine CH311.6112.4911.7412.3512.3811.099.07 CH246.2547.0745.7446.7747.1046.9647.19a See footnotes for Table1.b2J PC)3Hz.c Reference material;see text.For D2O solutions there is no accepted reference for carbon chemical shifts.We suggest the addition of a drop of methanol,and the position of its signal to be defined as49.50ppm;on this basis,the entries in Table2were recorded.The chemical shifts thus obtained are,on the whole,very similar to those for the other solvents. Alternatively,we suggest the use of dioxane when the methanol peak is expected to fall in a crowded area of the spectrum.We also report the chemical shifts of sodium formate(171.67ppm),sodium acetate(182.02and 23.97ppm),sodium carbonate(168.88ppm),sodium bicarbonate(161.08ppm),and sodium3-(trimethylsilyl)-propanesulfonate[54.90,19.66,15.56(methylenes1,2, and3,respectively),and-2.04ppm(methyls)],in D2O. Temperature Dependence of HDO Chemical Shifts.We recorded the1H spectrum of a sample of D2O, containing a crystal of sodium3-(trimethylsilyl)propane-sulfonate as reference,as a function of temperature.The data are shown in Figure1.The solid line connecting the experimental points corresponds to the equation which reproduces the measured values to better than1 ppb.For the0-50o C range,the simplergives values correct to10ppb.For both equations,T is the temperature in°C.Acknowledgment.Generous support for this work by the Minerva Foundation and the Otto Mayerhoff Center for the Study of Drug-Receptor Interactions at Bar-Ilan University is gratefully acknowledged.JO971176Vδ)5.060-0.0122T+(2.11×10-5)T2(1)δ)5.051-0.0111T(2)Notes .Chem.,Vol.62,No.21,19977515。
2021年-核磁谱图NMR常见溶剂峰杂质峰分析
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)2SO C6D6CD3CN CD3OH D2O溶剂峰—7.26 2.05 2.497.16 1.94 3.31 4.80水峰— 1.56 2.84 3.330.40 2.13 4.87—乙酸— 2.10 1.96 1.91 1.55 1.96 1.99 2.08丙酮— 2.17 2.09 2.09 1.55 2.08 2.15 2.22乙腈— 2.10 2.05 2.07 1.55 1.96 2.03 2.06苯—7.367.367.377.157.377.33—叔丁醇 CH3 1.28 1.18 1.11 1.05 1.16 1.40 1.24 OH—— 4.19 1.55 2.18——叔丁基甲醚CCH3 1.19 1.13 1.11 1.07 1.14 1.15 1.21OCH3 3.22 3.13 3.08 3.04 3.13 3.20 3.22氯仿—7.268.028.32 6.157.587.90—环己烷— 1.43 1.43 1.40 1.40 1.44 1.45—1,2- 二氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78—二氯甲烷— 5.30 5.63 5.76 4.27 5.44 5.49—乙醚CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17 CH2(q) 3.48 3.41 3.38 3.26 3.42 3.49 3.56二甲基甲酰胺CH8.027.967.957.637.927.797.92CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3 2.88 2.78 2.73 1.86 2.77 2.86 2.85二甲基亚砜— 2.62 2.52 2.54 1.68 2.50 2.65 2.71二氧杂环— 3.71 3.59 3.57 3.35 3.60 3.66 3.75乙醇CH3(t) 1.25 1.12 1.060.96 1.12 1.19 1.17 CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65 OH(s) 1.32 3.39 3.63— 2.47——乙酸乙酯 CH3CO 2.05 1.97 1.99 1.65 1.97 2.01 2.07 OCH2(q) 4.12 4.05 4.03 3.89 4.06 4.09 4.14 CH3(t) 1.26 1.20 1.170.92 1.20 1.24 1.24甲乙酮 CH3CO 2.14 2.07 2.07 1.58 2.06 2.12 2.19 CH2(q) 2.46 2.45 2.43 1.81 2.43 2.50 3.18 CH3(t) 1.060.960.910.850.96 1.01 1.26乙二醇— 3.76 3.28 3.34 3.41 3.51 3.59 3.65润滑脂 CH3(m)0.860.87—0.920.860.88—CH2(br) 1.26 1.29— 1.36 1.27 1.29—正己烷 CH3(t)0.880.880.860.890.890.90—CH2 (m) 1.26 1.28 1.25 1.24 1.28 1.29—甲醇CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH 1.09 3.12 4.01 2.16——正戊烷 CH3(t)0.880.880.860.870.890.90—CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29—异丙醇 CH3(d) 1.22 1.10 1.040.95 1.09 1.50 1.17 CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02硅脂—0.070.13—0.290.080.10—四氢呋喃 CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O 3.76 3.63 3.60 3.57 3.64 3.71 3.74甲苯CH3 2.36 2.32 2.30 2.11 2.33 2.32—CH （ o/p）7.177.207.187.027.307.16—CH （ m） 7.257.207.257.137.307.16—三乙基胺 CH3 1.030.960.930.960.96 1.050.99 CH2 2.53 2.45 2.43 2.40 2.45 2.58 2.57石油醚—0.5-1.50.6-1.9—————。
NMR常见溶剂峰和水峰
的耦合常数,H2O和交换了D的HOD上的1H产生的即水峰的化学位移
氯仿：小、中小、中等极性
DMSO：芳香系统日光下自然显色、紫外荧光;对于酚羟基能够出峰;芳香化合物还是芳香甙,都为首选;
吡啶：极性大的,特别是皂甙
对低、中极性的样品,最常采用氘代氯仿作溶剂,因其价格远低于其它氘代试剂;极性大的化合物可采用氘代丙酮、重水等;
针对一些特殊的样品,可采用相应的氘代试剂：如氘代苯用于芳香化合物、芳香高聚物、氘代二甲基亚砜用于某些在一般溶剂中难溶的物质、氘代吡啶用于难溶的酸性或芳香化合物等;
丙酮：中等极性
甲醇：极性大
氯仿—甲醇：
石：乙5；1小极性
石：丙2：1——1：1中等极性
氯仿：甲醇6：1极性以上含有一个糖
2：1含有两个糖
含有糖的三萜皂甙：一般用吡啶
常见溶剂的化学位移
常见溶剂的1H在不同氘代溶剂中的化学位移值
常见溶剂的化学位移
13
核磁知识NMR一：样品量的选择氢谱,氟谱,碳谱至少需要
5mg.1H-1HCOSY,1H-1HNOESY,1H-13CHMBC,1H-13CHSQC需要10-15mg.碳谱需要30mg.
二：如何选择氘代溶剂
常用氘代溶剂:CDCl3,DMSO,D2O,CD3OD.特殊氘代溶剂:CD3COCD3,C6D6,CD3CN;
极性较大的化合物可以选择用D2O或CD3OD,如果想要观察活泼氢切记不能选择D2O和CD3OD;CDCl3为人民币2-3元,D2O为人民币6元,DMSO为人民币10元,CD3OD为人民币30元;Solvent化学位移ppm水峰位移
ppmCDCl37.261.56DMSO2.503.33CD3OD3.314.87D2O4.79CD3COCD32.052.84。
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NMR Chemical Shifts of Common Laboratory Solvents as Trace Impurities Hugo E.Gottlieb,*Vadim Kotlyar,andAbraham Nudelman*Department of Chemistry,Bar-Ilan University,Ramat-Gan52900,IsraelReceived June27,1997In the course of the routine use of NMR as an aid for organic chemistry,a day-to-day problem is the identifica-tion of signals deriving from common contaminants (water,solvents,stabilizers,oils)in less-than-analyti-cally-pure samples.This data may be available in the literature,but the time involved in searching for it may be considerable.Another issue is the concentration dependence of chemical shifts(especially1H);results obtained two or three decades ago usually refer to much more concentrated samples,and run at lower magnetic fields,than today’s practice.We therefore decided to collect1H and13C chemical shifts of what are,in our experience,the most popular “extra peaks”in a variety of commonly used NMR solvents,in the hope that this will be of assistance to the practicing chemist.Experimental SectionNMR spectra were taken in a Bruker DPX-300instrument (300.1and75.5MHz for1H and13C,respectively).Unless otherwise indicated,all were run at room temperature(24(1°C).For the experiments in the last section of this paper,probe temperatures were measured with a calibrated Eurotherm840/T digital thermometer,connected to a thermocouple which was introduced into an NMR tube filled with mineral oil to ap-proximately the same level as a typical sample.At each temperature,the D2O samples were left to equilibrate for at least 10min before the data were collected.In order to avoid having to obtain hundreds of spectra,we prepared seven stock solutions containing approximately equal amounts of several of our entries,chosen in such a way as to prevent intermolecular interactions and possible ambiguities in assignment.Solution1:acetone,tert-butyl methyl ether,di-methylformamide,ethanol,toluene.Solution2:benzene,di-methyl sulfoxide,ethyl acetate,methanol.Solution3:acetic acid,chloroform,diethyl ether,2-propanol,tetrahydrofuran. Solution4:acetonitrile,dichloromethane,dioxane,n-hexane, HMPA.Solution5:1,2-dichloroethane,ethyl methyl ketone, n-pentane,pyridine.Solution6:tert-butyl alcohol,BHT,cyclo-hexane,1,2-dimethoxyethane,nitromethane,silicone grease, triethylamine.Solution7:diglyme,dimethylacetamide,ethyl-ene glycol,“grease”(engine oil).For D2O.Solution1:acetone, tert-butyl methyl ether,dimethylformamide,ethanol,2-propanol. Solution2:dimethyl sulfoxide,ethyl acetate,ethylene glycol, methanol.Solution3:acetonitrile,diglyme,dioxane,HMPA, pyridine.Solution4:1,2-dimethoxyethane,dimethylacetamide, ethyl methyl ketone,triethylamine.Solution5:acetic acid,tert-butyl alcohol,diethyl ether,tetrahydrofuran.In D2O and CD3OD nitromethane was run separately,as the protons exchanged with deuterium in presence of triethylamine.ResultsProton Spectra(Table1).A sample of0.6mL of the solvent,containing1µL of TMS,1was first run on its own.From this spectrum we determined the chemical shifts of the solvent residual peak2and the water peak. It should be noted that the latter is quite temperature-dependent(vide infra).Also,any potential hydrogen-bond acceptor will tend to shift the water signal down-field;this is particularly true for nonpolar solvents.In contrast,in e.g.DMSO the water is already strongly hydrogen-bonded to the solvent,and solutes have only a negligible effect on its chemical shift.This is also true for D2O;the chemical shift of the residual HDO is very temperature-dependent(vide infra)but,maybe counter-intuitively,remarkably solute(and pH)independent. We then added3µL of one of our stock solutions to the NMR tube.The chemical shifts were read and are presented in Table 1.Except where indicated,the coupling constants,and therefore the peak shapes,are essentially solvent-independent and are presented only once.For D2O as a solvent,the accepted reference peak(δ)0)is the methyl signal of the sodium salt of3-(trimeth-ylsilyl)propanesulfonic acid;one crystal of this was added to each NMR tube.This material has several disadvan-tages,however:it is not volatile,so it cannot be readily eliminated if the sample has to be recovered.In addition, unless one purchases it in the relatively expensive deuterated form,it adds three more signals to the spectrum(methylenes1,2,and3appear at2.91,1.76, and0.63ppm,respectively).We suggest that the re-sidual HDO peak be used as a secondary reference;we find that if the effects of temperature are taken into account(vide infra),this is very reproducible.For D2O, we used a different set of stock solutions,since many of the less polar substrates are not significantly water-soluble(see Table1).We also ran sodium acetate and sodium formate(chemical shifts: 1.90and8.44ppm, respectively).Carbon Spectra(Table2).To each tube,50µL of the stock solution and3µL of TMS1were added.The solvent chemical shifts3were obtained from the spectra containing the solutes,and the ranges of chemical shifts(1)For recommendations on the publication of NMR data,see: IUPAC Commission on Molecular Structure and Spectroscopy.Pure Appl.Chem.1972,29,627;1976,45,217.(2)I.e.,the signal of the proton for the isotopomer with one less deuterium than the perdeuterated material,e.g.,C H Cl3in CDCl3or C6D5H in C6D6.Except for CHCl3,the splitting due to J HD is typically observed(to a good approximation,it is1/6.5of the value of the corresponding J HH).For CHD2groups(deuterated acetone,DMSO, acetonitrile),this signal is a1:2:3:2:1quintet with a splitting of ca.2 Hz.(3)In contrast to what was said in note2,in the13C spectra the solvent signal is due to the perdeuterated isotopomer,and the one-bond couplings to deuterium are always observable(ca.20-30Hz). Figure1.Chemical shift of H DO as a function of tempera-ture..Chem.1997,62,7512-7515S0022-3263(97)01176-6CCC:$14.00©1997American Chemical Societyshow their degree of variability.Occasionally,in order to distinguish between peaks whose assignment was ambiguous,a further1-2µL of a specific substrate were added and the spectra run again.Table1.1H NMR Dataproton mult CDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent residual peak7.26 2.05 2.507.16 1.94 3.31 4.79 H2O s 1.56 2.84a 3.33a0.40 2.13 4.87acetic acid CH3s 2.10 1.96 1.91 1.55 1.96 1.99 2.08 acetone CH3s 2.17 2.09 2.09 1.55 2.08 2.15 2.22 acetonitrile CH3s 2.10 2.05 2.07 1.55 1.96 2.03 2.06 benzene CH s7.367.367.377.157.377.33tert-butyl alcohol CH3s 1.28 1.18 1.11 1.05 1.16 1.40 1.24 OH c s 4.19 1.55 2.18tert-butyl methyl ether CCH3s 1.19 1.13 1.11 1.07 1.14 1.15 1.21 OCH3s 3.22 3.13 3.08 3.04 3.13 3.20 3.22 BHT b ArH s 6.98 6.96 6.877.05 6.97 6.92OH c s 5.01 6.65 4.79 5.20ArCH3s 2.27 2.22 2.18 2.24 2.22 2.21ArC(CH3)3s 1.43 1.41 1.36 1.38 1.39 1.40chloroform CH s7.268.028.32 6.157.587.90 cyclohexane CH2s 1.43 1.43 1.40 1.40 1.44 1.451,2-dichloroethane CH2s 3.73 3.87 3.90 2.90 3.81 3.78 dichloromethane CH2s 5.30 5.63 5.76 4.27 5.44 5.49diethyl ether CH3t,7 1.21 1.11 1.09 1.11 1.12 1.18 1.17 CH2q,7 3.48 3.41 3.38 3.26 3.42 3.49 3.56 diglyme CH2m 3.65 3.56 3.51 3.46 3.53 3.61 3.67 CH2m 3.57 3.47 3.38 3.34 3.45 3.58 3.61OCH3s 3.39 3.28 3.24 3.11 3.29 3.35 3.37 1,2-dimethoxyethane CH3s 3.40 3.28 3.24 3.12 3.28 3.35 3.37 CH2s 3.55 3.46 3.43 3.33 3.45 3.52 3.60 dimethylacetamide CH3CO s 2.09 1.97 1.96 1.60 1.97 2.07 2.08 NCH3s 3.02 3.00 2.94 2.57 2.96 3.31 3.06NCH3s 2.94 2.83 2.78 2.05 2.83 2.92 2.90 dimethylformamide CH s8.027.967.957.637.927.977.92 CH3s 2.96 2.94 2.89 2.36 2.89 2.99 3.01CH3s 2.88 2.78 2.73 1.86 2.77 2.86 2.85 dimethyl sulfoxide CH3s 2.62 2.52 2.54 1.68 2.50 2.65 2.71 dioxane CH2s 3.71 3.59 3.57 3.35 3.60 3.66 3.75 ethanol CH3t,7 1.25 1.12 1.060.96 1.12 1.19 1.17 CH2q,7d 3.72 3.57 3.44 3.34 3.54 3.60 3.65OH s c,d 1.32 3.39 4.63 2.47ethyl acetate CH3CO s 2.05 1.97 1.99 1.65 1.97 2.01 2.07C H2CH3q,7 4.12 4.05 4.03 3.89 4.06 4.09 4.14CH2C H3t,7 1.26 1.20 1.170.92 1.20 1.24 1.24 ethyl methyl ketone CH3CO s 2.14 2.07 2.07 1.58 2.06 2.12 2.19C H2CH3q,7 2.46 2.45 2.43 1.81 2.43 2.50 3.18CH2C H3t,7 1.060.960.910.850.96 1.01 1.26 ethylene glycol CH s e 3.76 3.28 3.34 3.41 3.51 3.59 3.65“grease”f CH3m0.860.870.920.860.88CH2br s 1.26 1.29 1.36 1.27 1.29n-hexane CH3t0.880.880.860.890.890.90CH2m 1.26 1.28 1.25 1.24 1.28 1.29HMPA g CH3d,9.5 2.65 2.59 2.53 2.40 2.57 2.64 2.61 methanol CH3s h 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH s c,h 1.09 3.12 4.01 2.16nitromethane CH3s 4.33 4.43 4.42 2.94 4.31 4.34 4.40 n-pentane CH3t,70.880.880.860.870.890.90CH2m 1.27 1.27 1.27 1.23 1.29 1.292-propanol CH3d,6 1.22 1.10 1.040.95 1.09 1.50 1.17 CH sep,6 4.04 3.90 3.78 3.67 3.87 3.92 4.02 pyridine CH(2)m8.628.588.588.538.578.538.52 CH(3)m7.297.357.39 6.667.337.447.45CH(4)m7.687.767.79 6.987.737.857.87 silicone grease i CH3s0.070.130.290.080.10 tetrahydrofuran CH2m 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O m 3.76 3.63 3.60 3.57 3.64 3.71 3.74 toluene CH3s 2.36 2.32 2.30 2.11 2.33 2.32CH(o/p)m7.177.1-7.27.187.027.1-7.37.16CH(m)m7.257.1-7.27.257.137.1-7.37.16 triethylamine CH3t,7 1.030.960.930.960.96 1.050.99 CH2q,7 2.53 2.45 2.43 2.40 2.45 2.58 2.57a In these solvents the intermolecular rate of exchange is slow enough that a peak due to HDO is usually also observed;it appears at2.81and3.30ppm in acetone and DMSO,respectively.In the former solvent,it is often seen as a1:1:1triplet,with2J H,D)1Hz. b2,6-Dimethyl-4-tert-butylphenol.c The signals from exchangeable protons were not always identified.d In some cases(see note a),the coupling interaction between the CH2and the OH protons may be observed(J)5Hz).e In CD3CN,the OH proton was seen as a multiplet atδ2.69,and extra coupling was also apparent on the methylene peak.f Long-chain,linear aliphatic hydrocarbons.Their solubility in DMSO was too low to give visible peaks.g Hexamethylphosphoramide.h In some cases(see notes a,d),the coupling interaction between the CH3and the OH protons may be observed(J)5.5Hz).i Poly(dimethylsiloxane).Its solubility in DMSO was too low to give visible peaks.Notes .Chem.,Vol.62,No.21,19977513.Chem.,Vol.62,No.21,1997NotesTable2.13C NMR Data aCDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent signals77.16(0.0629.84(0.0139.52(0.06128.06(0.02 1.32(0.0249.00(0.01206.26(0.13118.26(0.02acetic acid CO175.99172.31171.93175.82173.21175.11177.21 CH320.8120.5120.9520.3720.7320.5621.03 acetone CO207.07205.87206.31204.43207.43209.67215.94 CH330.9230.6030.5630.1430.9130.6730.89 acetonitrile CN116.43117.60117.91116.02118.26118.06119.68 CH3 1.89 1.12 1.030.20 1.790.85 1.47 benzene CH128.37129.15128.30128.62129.32129.34tert-butyl alcohol C69.1568.1366.8868.1968.7469.4070.36 CH331.2530.7230.3830.4730.6830.9130.29 tert-butyl methyl ether OCH349.4549.3548.7049.1949.5249.6649.37 C72.8772.8172.0472.4073.1774.3275.62C C H326.9927.2426.7927.0927.2827.2226.60 BHT C(1)151.55152.51151.47152.05152.42152.85C(2)135.87138.19139.12136.08138.13139.09CH(3)125.55129.05127.97128.52129.61129.49C(4)128.27126.03124.85125.83126.38126.11CH3Ar21.2021.3120.9721.4021.2321.38C H3C30.3331.6131.2531.3431.5031.15C34.2535.0034.3334.3535.0535.36chloroform CH77.3679.1979.1677.7979.1779.44cyclohexane CH226.9427.5126.3327.2327.6327.961,2-dichloroethane CH243.5045.2545.0243.5945.5445.11 dichloromethane CH253.5254.9554.8453.4655.3254.78diethyl ether CH315.2015.7815.1215.4615.6315.4614.77 CH265.9166.1262.0565.9466.3266.8866.42 diglyme CH359.0158.7757.9858.6658.9059.0658.67 CH270.5171.0369.5470.8770.9971.3370.05CH271.9072.6371.2572.3572.6372.9271.63 1,2-dimethoxyethane CH359.0858.4558.0158.6858.8959.0658.67 CH271.8472.4717.0772.2172.4772.7271.49 dimethylacetamide CH321.5321.5121.2921.1621.7621.3221.09 CO171.07170.61169.54169.95171.31173.32174.57NCH335.2834.8937.3834.6735.1735.5035.03NCH338.1337.9234.4237.0338.2638.4338.76 dimethylformamide CH162.62162.79162.29162.13163.31164.73165.53 CH336.5036.1535.7335.2536.5736.8937.54CH331.4531.0330.7330.7231.3231.6132.03 dimethyl sulfoxide CH340.7641.2340.4540.0341.3140.4539.39 dioxane CH267.1467.6066.3667.1667.7268.1167.19 ethanol CH318.4118.8918.5118.7218.8018.4017.47 CH258.2857.7256.0757.8657.9658.2658.05 ethyl acetate C H3CO21.0420.8320.6820.5621.1620.8821.15 CO171.36170.96170.31170.44171.68172.89175.26CH260.4960.5659.7460.2160.9861.5062.32CH314.1914.5014.4014.1914.5414.4913.92 ethyl methyl ketone C H3CO29.4929.3029.2628.5629.6029.3929.49 CO209.56208.30208.72206.55209.88212.16218.43C H2CH336.8936.7535.8336.3637.0937.3437.27CH2C H37.868.037.617.918.148.097.87 ethylene glycol CH263.7964.2662.7664.3464.2264.3063.17“grease”CH229.7630.7329.2030.2130.8631.29n-hexane CH314.1414.3413.8814.3214.4314.45CH2(2)22.7023.2822.0523.0423.4023.68CH2(3)31.6432.3030.9531.9632.3632.73HMPA b CH336.8737.0436.4236.8837.1037.0036.46 methanol CH350.4149.7748.5949.9749.9049.8649.50c nitromethane CH362.5063.2163.2861.1663.6663.0863.22 n-pentane CH314.0814.2913.2814.2514.3714.39CH2(2)22.3822.9821.7022.7223.0823.38CH2(3)34.1634.8333.4834.4534.8935.302-propanol CH325.1425.6725.4325.1825.5525.2724.38 CH64.5063.8564.9264.2364.3064.7164.88 pyridine CH(2)149.90150.67149.58150.27150.76150.07149.18 CH(3)123.75124.57123.84123.58127.76125.53125.12CH(4)135.96136.56136.05135.28136.89138.35138.27 silicone grease CH3 1.04 1.40 1.38 2.10 tetrahydrofuran CH225.6226.1525.1425.7226.2726.4825.67 CH2O67.9768.0767.0367.8068.3368.8368.68 toluene CH321.4621.4620.9921.1021.5021.50C(i)137.89138.48137.35137.91138.90138.85CH(o)129.07129.76128.88129.33129.94129.91CH(m)128.26129.03128.18128.56129.23129.20CH(p)125.33126.12125.29125.68126.28126.29triethylamine CH311.6112.4911.7412.3512.3811.099.07 CH246.2547.0745.7446.7747.1046.9647.19a See footnotes for Table1.b2J PC)3Hz.c Reference material;see text.For D2O solutions there is no accepted reference for carbon chemical shifts.We suggest the addition of a drop of methanol,and the position of its signal to be defined as49.50ppm;on this basis,the entries in Table2were recorded.The chemical shifts thus obtained are,on the whole,very similar to those for the other solvents. Alternatively,we suggest the use of dioxane when the methanol peak is expected to fall in a crowded area of the spectrum.We also report the chemical shifts of sodium formate(171.67ppm),sodium acetate(182.02and 23.97ppm),sodium carbonate(168.88ppm),sodium bicarbonate(161.08ppm),and sodium3-(trimethylsilyl)-propanesulfonate[54.90,19.66,15.56(methylenes1,2, and3,respectively),and-2.04ppm(methyls)],in D2O. Temperature Dependence of HDO Chemical Shifts.We recorded the1H spectrum of a sample of D2O, containing a crystal of sodium3-(trimethylsilyl)propane-sulfonate as reference,as a function of temperature.The data are shown in Figure1.The solid line connecting the experimental points corresponds to the equation which reproduces the measured values to better than1 ppb.For the0-50o C range,the simplergives values correct to10ppb.For both equations,T is the temperature in°C.Acknowledgment.Generous support for this work by the Minerva Foundation and the Otto Mayerhoff Center for the Study of Drug-Receptor Interactions at Bar-Ilan University is gratefully acknowledged.JO971176Vδ)5.060-0.0122T+(2.11×10-5)T2(1)δ)5.051-0.0111T(2)Notes .Chem.,Vol.62,No.21,19977515。