Jump to content Jump to navigation menu

Nuclear magnetic resonance spectroscopy (NMR)

NMR spectroscopy has become one of the most important instruments in the field of structure determination of a wide variety of compounds. For example, NMR spectroscopy cannot only be used to determine molecular structures but also to get informations about the identity and purity of substances, molecular conformations and intermolecular interactions. Generally speaking, the method serves to investigate the electronic environment of individual atoms and thus provides insight into the interactions between neighbouring atoms. However, certain factors such as the solubility of the sample, the water content and viscosity of the solvent as well as the position of the solvent signals in the spectrum have to be taken into account, when selecting a suitable solvent.

To provide laboratories with support in carrying out such analyses, Carl ROTH offers a range of deuterated solvents, acids and bases as well as additional consumables for NMR spectroscopy.
414131744_650px.jpg

Advantages:

  • High degree of deuteration
  • Defined water content
  • Extremely cost effective
     

Application examples:

  • Routine tasks such as structure determination and identity verification in research and development laboratories
  • Elucidation of reaction mechanisms and metabolisms
  • For GC-MS or LC-MS as internal standards
 Compounds and solvents for NMR spectroscopy
 Accessories for NMR spectroscopy

6672
Trichloromethane/Chloroform D1
99,8 Atom%D, stabilised with Ag
from €38.60
6672_AE56
Methanol D4
99,8 Atom%D
from €85.90
6672_AE56
Deuterium oxide
99,9 Atom%D
from €48.30
6672_AE56
Dimethyl sulphoxide D6
99,8 Atom%D
from €65.50
HX58
NMR tube ROTILABO®
from €111.85
YA94
Sample stands for NMR tubes
from €99.60
6672_AE56
Pyridine D5
99,5 Atom%D
from €177.40
6672
Deuterium chloride 38 % solution in D2O
99,5 Atom%D
from €80.10
EP54
NMR tubes Scientific
from €92.20
Webshop_Platzhalter_Chem_LS
3-(Trimethylsilyl)propionic-2,2,3,3 acid sodium salt D4 (TSP-D4)
99 Atom%D
from €192.45
CP18
Tetramethylsilane
≥99,9 %, for NMR spectroscopy
from €40.75

NMR_Flyer_650px.jpg

NMR Spectroscopy Overview Flyer

NMR Chemical Shifts of Common Solvents as Trace Impurities

Download PDF

NMR Spectroscopy

Deuterated Compounds and Accessories

NMR Chemical Shifts of Common Solvents as Trace Impurities


These tables present the NMR shifts of commonly used solvents and impurities in organic synthesis and workup protocols measured in the 7 most frequently used deuterated solvents.

To simplify the identification of these solvents in NMR spectra and facilitate their adoption into chemical processes, we have compiled 1H and 13C NMR data for common laboratory solvents.
 
62480202_650px.jpg

1H NMR Chemical Impurity Shifts Table

Proton Mult. CDCl3 (CD3)2CO (CD3)2SO C6D6 CD3CN CD3OD D2O
Solvent residual
peak		 - - 7.26 2.05 2.50 7.16 1.94 3.31 4.79
H2O - s 1.56 2.84 3.33 0.40 2.13 4.87 -
Acetic acid CH3 s 2.10 1.96 1.91 1.55 1.96 1.99 2.08
Acetone CH3 s 2.17 2.09 2.09 1.55 2.08 2.15 2.22
Acetonitrile CH3 s 2.10 2.05 2.07 1,55 1.96 2.03 2.06
Benzene CH s 7.36 7.36 7.36 7.15 7.37 7.33 -
Benzyl alcohol CH
CH
CH2
OH		 m
m
d, 5.9
t, 5.9		 7.28−7.38
7.28−7.38
4.71
1.64		 7.29−7.37
7.20−7.25
4.63
4.16		 7.28−7.36
7.20−7.25
4.49
5.16		 -
-
-
-		 7.30−7.37
7.23−7.29
4.57
3.14		 7.30−7.36
7.22−7.26
4.59, s		 7.37−7.47
7.37−7.47
4.65, s
tert-Butanol CH3
OH		 s
s		 1.27
-		 1.18
3.22		 1.11
4.18		 1.05
1.55		 1.17
2.39		 1.22
-		 1.25
-
2-Butanone (MEK) CH3CO
CH2
CH2CH3		 s
q, 7
t, 7		 2.14
2.46
1.06		 2.07
2.45
0.96		 2.07
2.43
0.91		 1.58
1.81
0.85		 2.06
2.43
0.96		 2.12
2.50
1.01		 2.19
3.18
1.26
tert-Butyl methyl ether
(MTBE)		 CCH3
OCH3		 s
s		 1.19
3.22		 1.13
3.13		 1.11
3.08		 1.07
3.04		 1.14
3.13		 1.15
3.20		 1.21
3.22
Chlorobenzene CH m 7.22−7.36 7.31−7.42 7.32−7.45 - 7.29−7.41 7.25−7.37 7.33−7.46
Chloroform CH s 7.26 8.02 8.32 6.15 7.58 7.90 -
Cyclohexane CH2 s 1.43 1.43 1.40 1.40 1.44 1.45 -
Cyclopentyl methyl ether
(CPME) 		 CH
OCH3
CH2		 m
s
m		 3.78−3.82
3.28
1.50−1.74		 3.73−3.77
3.19
1.44−1.72		 3.71−3.76
3.15
1.42−1.67		 -
-
-		 3.74−3.78
3.19
1.48−1.70		 3.80−3.85
3.26
1.50−1.77		 3.94−3.99
3.30
1.51−1.86
1,2-Dichloroethane CH2 s 3.73 3.87 3.90 2.90 3.81 3.78 -
Dichloromethane CH2 s 5.30 5.63 5.76 4.27 5.44 5.49 -
Diethyl ether CH3
CH2		 t, 7
q, 7		 1.21
3.48		 1.11
3.41		 1.09
3.38		 1.11
3.26		 1.12
3.42		 1.18
3.49		 1.17
3.56
1,2-Dimethoxyethane CH3
CH2		 s
s		 3.40
3.55		 3.28
3.46		 3.24
3.43		 3.12
3.33		 3.28
3.45		 3.35
3.52		 3.37
3.60
Dimethylacetamide CH3CO
NCH3
NCH3		 s
s
s		 2.09
3.02
2.94		 1.97
3.00
2.83		 1.96
2.94
2.78		 1.60
2.54
2.05		 1.97
2.96
2.83		 2.07
3.30
2.92		 2.08
3.06
2.90
Dimethylformamide CH
CH3
CH3		 s
s
s		 8.02
2.96
2.88		 7.96
2.94
2.78		 7.95
2.89
2.73		 7.63
2.36
1.86		 7.92
2.89
2.77		 7.97
2.99
2.86		 7.92
3.01
2.85
Dimethyl sulfoxide CH3 s 2.62 2.52 2.54 1.68 2.50 2.65 2.71
Dioxane CH2 s 3.71 3.59 3.57 3.35 3.60 3.66 3.75
Ethanol CH3
CH2
OH		 t, 7
q, 7
s		 1.25
3.72
1.32		 1.12
3.57
3.39		 1.06
3.44
4.63		 0.96
3.34
-		 1.12
3.54
2.47		 1.19
3.60
-		 1.17
3.65
-
Ethyl acetate CH3CO
CH2CH3
CH2CH3		 s
q, 7
t, 7		 2.05
4.12
1.26		 1.97
4.05
1.20		 1.99
4.03
1.17		 1.65
3.89
0.92		 1.97
4.06
1.20		 2.01
4.09
1.24		 2.07
4.14
1.24
Ethylene glycol CH s 3.67 3.28 3.34 3.41 3.51 3.59 3.65
“Grease” CH3
CH2		 m
brs		 0.86
1.26		 0.87
1.29		 -
-		 0.92
1.36		 0.86
1.27		 0.88
1.29		 -
-
n-Hexane CH3
CH2		 t
m		 0.88
1.26		 0.88
1.28		 0.86
1.25		 0.89
1.24		 0.89
1.28		 0.90
1.29		 -
-
Methanol CH3
OH		 s
s		 3.49
1.09		 3.31
3.12		 3.16
4.01		 3.07
-		 3.28
2.16		 3.34
-		 3.34
-
Nitromethane CH3 s 4.33 4.43 4.42 2.94 4.31 4.34 4.40
n-Pentane CH3
CH2		 t, 7
m		 0.88
1.27		 0.88
1.27		 0.86
1.27		 0.87
1.23		 0.89
1.29		 0.90
1.29		 -
-
2-Propanol CH
CH3
OH		 septd, 6.1, 4.3
d, 6.1
d, 4.3		 4.03, sept (6.1)
1.21
-		 3.84−3.95, m
1.10
3.39		 3.77
1.04
4.34		 -
-
-		 3-89
1.09
2.51		 3.92, sept (6.1)
1.15
-		 4.02, sept (6.2)
1.18
-
Pyridine CH (2)
CH (3)
CH (4)		 m
m
m		 8.62
7.29
7.68		 8.58
7.35
7.76		 8.58
7.39
7.79		 8.53
6.66
6.98		 8.57
7.33
7.73		 8.53
7.44
7.85		 8.52
7.45
7.87
Silicone grease CH3 s 0.07 0.13 - 0.29 0.08 0.10 -
Tetrahydrofuran CH2
CH2O		 m
m		 1.85
3.76		 1.79
3.63		 1.76
3.60		 1.40
3.57		 1.80
3.64		 1.87
3.71		 1.88
3.74
Toluene CH3
CH (o/p)
CH (m)		 s
m
m		 2.36
7.17
7.25		 2.32
7.1−7.2
7.1−7.2		 2.30
7.18
7.25		 2.11
7.02
7.13		 2.33
7.1−7.3
7.1−7.3		 2.32
7.16
7.16		 -
-
-
Triethylamine CH3
CH2		 t, 7
q, 7		 1.03
2.53		 0.96
2.45		 0.93
2.43		 0.96
2.40		 0.96
2.45		 1.05
2.58		 0.99
2.57
Xylenes
o-Xylene CH
CH3		 m
s		 7.08−7.14
2.26		 7.03−7.12
2.23		 7.04−7.14
2.21		 -
-		 7.05−7.15
2.25		 7.01−7.10
2.24		 -
-
m-Xylene CH (5)
CH (2,4,6)
CH3		 t, 7.5
m
s		 7.15
6.96−7.00
2.32		 7.15
6.94−6.99
2.27		 7.13
6.95−6.99
2.26		 -
-
-		 7.13
6.96−7.01
2.28		 7.08
6.92−6.97
2.27		 7.24
7.07−7.14
2.31
p-Xylene CH
CH3		 s
s		 7.06
2.31		 7.05
2.26		 7.05
2.24		 -
-		 7.06
2.27		 7.02
2.26		 7.18
2.30

13C NMR Chemical Impurity Shifts Table

  Carbon CDCl3 (CD3)2CO (CD3)2SO C6D6 CD3CN CD3OD D2O
Solvent residual peak - 77.16 ±0.06 29.84 ±0.01
206.26 ±0.13		 39.52 ±0.06 128.06 ±0.02 1.32 ±0.02
118.26 ±0.02		 49.00 ±0.01 -
Acetic acid CO
CH3		 175.99
20.81		 172.31
20.51		 171.93
20.95		 175.82
20.37		 173.21
20.73		 175.11
20.56		 177.21
21.03
Acetone CN
CH3		 207.07
30.92		 205.87
30.60		 206.31
30.56		 204.43
30.14		 207.43
30.91		 209.67
30.67		 215.94
30.89
Acetonitrile CN
CH3		 116.43
1.89		 117.60
1.12		 117.91
1.03		 116.20
0.20		 118.26
1.79		 118.06
0.85		 119.68
1.47
Benzene CH 128.37 129.15 128.30 128.62 129.32 129.34 -
Benzyl alcohol C (1)
CH (3,5)
CH (4)
CH (2,6)
CH2		 140.98
128.54
127.61
126.98
65.31		 143.52
128.92
127.55
127.35
64.68		 142.44
127.92
126.50
126.31
62.82		 -
-
-
-
-		 143.17
129.26
127.97
127.69
64.76		 142.74
129.37
128.28
128.01
65.28		 140.84
129.34
128.43
128.06
64.51
tert-Butanol C
CH3		 69.15
313.25		 68.13
30.72		 66.88
30.88		 68.19
30.47		 68.74
30.68		 69.40
30.91		 70.36
30.29
2-Butanone (MEK) CH3CO
CO
CH2
CH2CH3		 29.49
209.56
36.89
7.86		 29.30
208.30
36.75
8.03		 29.26
208.70
35.83
7.61		 28.56
206.55
36.36
7.91		 29.60
209.88
37.09
8.14		 29.39
212.16
37.34
8.09		 29.49
218.43
37.27
7.87
tert-Butyl methyl ether
(MTBE)		 OCH3
C
CCH3		 49.45
72.87
26.99		 49.35
72.81
27.24		 48.70
72.04
26.79		 49.19
72.40
27.09		 49.52
73.17
27.28		 49.66
74.32
27.22		 49.37
75.62
26.60
Chlorobenzene C (1)
CH (3,5)
CH (2,6)
CH (4)		 134.29
129.71
128.62
126.43		 134.63
130.94
129.30
127.65		 133.00
130.20
128.30
126.92		 -
-
-
-		 134.74
131.10
129.45
127.83		 135.31
131.00
129.56
127.73		 -
-
-
-
Chloroform CH 77.36 79.19 79.16 77.79 79.17 79.44 -
Cyclohexane CH2 26.94 27.51 26.33 27.23 27.63 27.96 -
Cyclopentyl methyl ether
(CPME) 		 CH
CH3
CH2 (2,5)
CH2 (3,4)		 83.03
54.30
31.97
23.55		 83.35
56.18
32.51
24.14		 81.92
55.47
31.35
23.05		 -
-
-
-		 83.62
56.38
32.63
24.28		 84.47
56.55
32.85
24.45		 84.40
56.04
31.87
23.61
1,2-Dichloroethane CH2 43.50 45.25 45.02 43.59 45.54 45.11 -
Dichloromethane CH2 53.52 54.95 54.84 53.46 55.32 54.78 -
Diethyl ether CH3
CH2		 15.20
65.91		 15.75
66.12		 15.12
62.05		 15.46
65.94		 15.63
66.32		 15.46
66.88		 14.77
66.42
1,2-Dimethoxyethane CH3
CH2		 59.08
71.84		 58.45
72.47		 58.01
17.07		 58.68
72.21		 58.89
72.47		 59.06
72.72		 58.67
71.49
Dimethylacetamide CH3
CO
NCH3
NCH3		 21.53
171.07
35.28
38.13		 21.51
170.61
34.89
37.92		 21.29
169.54
37.38
34.42		 21.16
169.95
34.67
37.03		 21.76
171.31
35.17
38.26		 21.32
173.32
35.50
38.43		 21.09
174.57
35.03
38.76
Dimethylformamide C
CH3
CH3		 162.62
36.50
31.45		 162.79
36.15
31.03		 162.29
35.73
30.73		 162.13
35.25
30.72		 163.31
36.57
31.32		 164.73
36.89
31.61		 165.53
37.54
32.03
Dimethyl sulfoxide CH3 40.76 41.23 40.45 40.03 41.31 40.45 39.39
Dioxane CH2 67.14 67.60 66.36 67.16 67.72 68.11 67.19
Ethanol CH3
CH2		 18.41
58.28		 18.89
57.72		 18.51
56.07		 18.72
57.86		 18.80
57.96		 18.40
58.26		 17.47
58.05
Ethyl acetate CH3CO
CO
CH2
CH2		 21.04
171.36
60.49
14.19		 20.83
170.96
60.56
14.50		 20.68
170.31
59.74
14.40		 20.56
170.44
60.21
14.19		 21.16
171.68
60.98
14.54		 20.88
172.89
61.50
14.49		 21.15
175.26
62.32
13.92
Ethylene glycol CH2 63.79 64.26 62.76 64.34 64.22 64.30 63.17
“Grease” CH2 29.76 30.73 29.20 30.21 30.86 31.29 -
n-Hexane CH3
CH2 (2)
CH2 (3)		 14.14
22.70
31.64		 14.34
23.28
32.30		 13.88
22.05
30.95		 14.32
23.04
31.96		 14.43
23.40
32.36		 14.45
23.68
32.73		 -
-
-
Methanol CH3 50.41 49.77 48.59 49.97 49.90 49.86 49.50
Nitromethane CH3 62.50 53.21 63.28 61.16 63.66 63.08 63.22
n-Pentane CH3
CH2 (2)
CH2 (3)		 14.08
22.38
34.16		 14.29
22.98
34.83		 13.28
21.70
33.48		 14.25
22.81
34.45		 14.37
23.08
34.89		 14.39
23.38
35.30		 -
-
-
2-Propanol CH3
CH		 25.14
64.50		 25.67
63.85		 25.43
64.92		 25.18
64.23		 25.55
64.30		 25.27
64.71		 24.38
64.88
Pyridine CH (2)
CH (3)
CH (4)		 149.90
123.75
135.96		 150.67
124.57
136.56		 149.58
123.84
136.05		 150.27
123.58
123.28		 150.76
127.76
136.89		 150.07
125.53
138.35		 149.18
125.12
138.27
Silicone grease CH3 1.04 1.40 - 1.38 - 2.10 -
Tetrahydrofuran CH2
CH2O		 25.62
67.97		 26.15
68.07		 25.14
67.03		 25.72
67.80		 26.27
68.33		 26.48
68.83		 25.67
68.68
Toluene CH3
CH (i)
CH (o)
CH (m)
CH (p)		 21.46
137.89
129.07
128.26
125.33		 21.46
138.48
129.76
129.03
126.12		 20.99
137.35
128.88
128.18
125.29		 21.10
137.91
129.33
128.56
125.68		 21.50
138.90
129.94
129.23
126.28		 21.50
138.85
129.91
129.20
126.29		 -
-
-
-
-
Triethylamine CH3
CH2		 11.61
46.25		 12.49
47.07		 11.74
45.74		 12.35
46.77		 12.38
47.10		 11.09
46.96		 9.07
47.19
Xylenes
o-Xylene C (1,2)
CH (3,6)
CH (4,5)
CH3		 136.49
129.59
125.79
19.71		 137.03
130.28
126.58
19.68		 135.91
129.29
125.61
19.24		 -
-
-
-		 137.51
130.46
126.78
19.79		 137.37
130.47
126.81
19.77		 -
-
-
-
m-Xylene C (1,3)
CH (2)
CH (5)
CH (4,6)
CH3		 137.78
129.91
128.15
126.04
21.33		 138.34
130.52
128.93
126.78
21.32		 137.07
129.51
127.98
125.83
20.83		 -
-
-
-
-		 138.80
130.71
129.16
126.95
21.40		 138.79
130.70
129.13
126.99
21.42		 -
-
-
-
-
p-Xylene C (1,4)
CH (2,3,5,6)
CH3		 134.67
128.92
20.94		 135.27
129.65
20.94		 134.03
128.69
20.49		 -
-
-		 135.68
129.85
21.00		 135.71
129.84
21.02		 -
-
-

References

  1. Gottlieb, H. E.; Kotlyar, V.; Nudelman, A.; J.Org.Chem. , 1997, 62 , 7512.
  2. Babij, N. R.; McCusker, E. O.; Whiteker, G. T.; Canturk, B.; Choy, N.; Creemer, L. C.; Amicis, C. V. D.; Hewlett, N. M.; Johnson, P. L.; Knobelsdorf, J. A.; Li, F.; Lorsbach, B. A.; Nugent, B. M.; Ryan, S. J.; Smith, M. R.; Yang, Q. Org. Process Res. Dev. 2016, 20 , 661– 667.