NMR Experiment Guide
NMR experiments currently available in automation mode.
| Parameter Set | Default Time | Description | Special Instructions | Pulse Sequence |
| PROTON | 1min30s | 1D 1H, uses 30° pulse for reliable integrals. | Change NS to increase signal if desired. Switch to night queue if increasing length over 20 min. | zg30 |
| C13CPD32 | 1min56s | 1D 13C, 32 scans. Uses decoupling during delay and acquisition for increased sensitivity. Provides OK S/N for ~25 mg samples. Carbons without attached protons will be weaker. | Change NS to increase signal if desired. Do not set length longer than 30 min on NEO400. | zgpg30 |
| C13CPD | 59min | Same as C13CPD32 but runs for 1 hr. Night queue only. Provides OK S/N for ~6 mg samples. | Check available night queue time before submitting. | zgpg30 |
| C13DEPT135 | 17min55s | 1D 13C DEPT135. Sensitivity enhanced and multiplicity edited. Carbons without attached protons are not observed. CH and CH3 carbons should be positive and CH2 carbons should be negative (or backwards if phased upside-down). Night queue only. | Check available night queue time before submitting. | deptsp135 |
| WATERSUP1 | 2min17s | 1D 1H with largest peak automatically suppressed (usually should be solvent). Will not suppress multiple signals (such as for ETOH or THF). 90° pulse width. | Do not use unless there is a large, undesirable peak in spectrum. Peaks near the large peak may also be affected. | noesygppr1d |
| PROB11DEC | 54s | 1D 1H with 11B decoupled. | Set O2p right on resonance with 11B signal. | zgig |
PROF19DEC (400s only) |
54s | 1D 1H with 19F decoupled. | Set O2p right on resonance with 19F signal. | zgig |
| PROP31DEC | 54s | 1D 1H with 31P decoupled. | Set O2p right on resonance with 31P signal. | zgig |
SAPPHIRE pureshift1H (NEO400 only) |
6min41s | 1D 1H (reconstructed) with 1H-1H couplings removed (pure shift). Geminal protons will still be doublets. Provides OK S/N for ~6 mg samples. | Note the much-lower sensitivity compared to PROTON. HSQC_PURESHIFT may provide better sensitivity. | sapphire_ZS_AG |
| PROTON BIGSW | 1min17s | Same as PROTON but the window is 50 ppm wide and centered at -5 ppm. | zg30 | |
| PROTONT1 | 25min14s | Inversion-recovery measurement to determine 1H T1s. | Data can be analyzed with the command "t1guide" in Topspin. | t1ir |
F19 (400s only) |
35s | 1D F19, no decoupling. | Probe background around -170 ppm can be removed with linear prediction if desired. | zg |
F19CPD (400s only) |
35s | 1D F19, 1H decoupling during acquisition. | Probe background around -170 ppm can be removed with linear prediction if desired. | zgig |
F19ECHO (400s only) |
4min38s | 1D F19 with background-suppressing echo, no decoupling, and a 30° pulse width for more accurate integrals. | Collect a F19 spectrum as well. F19 signals with strong couplings (CF2H, geminal CF2s) can be badly distorted with the echo. Do not rely on this spectrum alone for quantification. | zgsezr |
F19ECHO IG (400s only) |
4min38s | 1D F19 with background-suppressing echo, 1H decoupling during acquisition, and a 30° pulse width for more accurate integrals. | Collect a F19CPD spectrum as well. F19 signals with strong couplings (CF2H, geminal CF2s) can be badly distorted with the echo. Do not rely on this spectrum alone for quantification. | zgigsezr |
F19T1IR (400s only) |
9min4s | Inversion-recovery measurement to determine 19F T1s. | Data can be analyzed with the command "t1guide" in Topspin. | t1irig |
| P31 | 1min31s | 1D 31P, uses 30° pulse for reliable integrals. No decoupling. | Change NS to increase signal if desired. Switch to night queue if increasing length over 20 min. | zg30 |
| P31CPD | 51s | 1D 31P, uses 30° pulse for reliable integrals. Uses decoupling during delay and acquisition for increased sensitivity. | zgpg30 | |
P31 CRP20 |
1min32s | 1D 31P, uses 30° pulse for reliable integrals. Uses decoupling during delay and acquisition for increased sensitivity. Uses chirped decoupling to decouple larger bandwidth of protons (from about 10 ppm to -30 ppm). | Use this if you need to decouple protons both in the normal 0-8 ppm range but also down to about -30 ppm. | zgpg30 |
| COSYPH | 1hr27min | 2D 1H-1H COSY (COrrelation SpectroscopY). Night queue only. | cosyph | |
COSY PHPR |
1hr28min | 2D COSYPH with automatic solvent suppression. Does not suppress multiple signals. Night queue only. | Set O1P to the position of your solvent peak (only on AV400 and AV500). Only use this if there is a large, undesirable peak in spectrum. Peaks near the large peak may also be affected. | cosyphpr |
NOESY GPPHSW |
49min53s | 2D NOESY (Nuclear Overhauser Effect SpectroscopY). Measures 1H-1H through-space contacts and chemical exchange. Default mixing time D8 of 0.3 sec (but can be modified). With positive diagonal peaks, negative cross peaks indicate NOE or chemical exchange. Night queue only. | noesygpph | |
ROESY PHSW_N |
47min46s | 2D ROESY (ROtating frame noESY). Measures 1H-1H through-space contacts and chemical exchange like NOESY. With positive diagonal peaks, positive cross peaks indicate NOE contacts, and negative cross peaks indicate chemical exchange. Night queue only. | Can be better than NOESY for molecules of approximately 1000 Da. | roesyphpp.2 |
HSQCEDETGP-SISP.2_ADIA (NEO400 and AV500 only) |
55min51s | 2D 1H-13C HSQC (Heteronuclear Single Quantum Coherence). Multiplicity-edited so CH and CH3 peaks are positive and CH2 are negative. | hsqcedetgpsisp.2 | |
HSQC PURESHIFT (NEO400 and AV500 only) |
1hr7min | 2D 1H-13C HSQC (Heteronuclear Single Quantum Coherence). Multiplicity-edited so CH and CH3 peaks are positive and CH2 are negative. 1H signals are pure shift (1H-1H couplings removed) using BIRD decoupling for improved signal and resolution. Night queue only. | hsqcedetgpsisp2.3_bbhd | |
| HMBCETGP-L3ND_13C | 1hr25min | 2D 1H-13C HMBC (Heteronuclear Multiple Bond Correlation). Gives 2+ bond correlations between 13C and 1H. 3-bond correlations are often stronger than 2- and 4-bond. Night queue only. | hmbcetgpl3nd | |
1H_19F HMBC_2D (400s only) |
1hr25min | 2D 1H-19F HMBC (Heteronuclear Multiple Bond Correlation). Night queue only. | You should set the 1sw (window) and o2p (center frequency) to cover the range of signals in your 19F 1D but not much larger. | hmbcetgpl3nd |
1H_19F HOESY_2D (NEO400 only) |
3hr7min | 2D 1H-19F HOESY (Heteronuclear Overhauser Effect SpectroscopY). Gives 19F-1H through-space contacts. Night queue only. | You should set the 1sw (window) and o2p (center frequency) to cover the range of signals in your 19F 1D but not much larger. | hoesyetgpsp.2.nodec |
F19COSY (NEO400 only) |
1hr29min | 2D 19F-19F COSY (COrrelation SpectroscopY). Night queue only. | Set 1sw, 2sw (window), o1p and o2p (center frequencies) to cover range of 19F and not larger. Be careful--19F-19F J couplings are sometimes very different from expected based on 1H-1H couplings due to geometry differences. | cosygpqf |
F19NOESY (NEO400 only) |
4hr9min | 2D NOESY (Nuclear Overhauser Effect SpectroscopY). Measures 19F-19F through-space contacts. Night queue only. | Set 1sw, 2sw (window), o1p and o2p (center frequencies) to cover range of 19F and not larger. | noesyetgp.sp |
1H_31P HMBC_2D |
42min50s | 2D 1H-31P HMBC (Heteronuclear Multiple Bond Correlation). Night queue only. | You should set the 1sw (window) and o2p (center frequency) to cover the range of signals in your 31P 1D but not much larger. | hmbcetgpl3nd |
DOSY (NEO400 and AV500 only) |
20min36s | Diffusion Ordered SpectroscopY. Separates 1H NMR signals by diffusion coefficients. Good for mixtures and for determining rough molecular weights. | Use a dilute solution and a medium viscosity solvent like H2O. Analysis is best done using Topspin, not MNova. | ledbpgp2s |
DOSY_CC (NEO400 and AV500 only) |
20min42s | Like DOSY but with convection compensation for more accurate results, especially for low viscosity solvents. | Use a dilute solution and a medium viscosity solvent like H2O. Analysis is best done using Topspin, not MNova. | dstebpgp3s |
PROJECTED DOSY_CC (NEO400 only) |
17min23s | Like DOSY_CC but with compensation for chemical exchange effects. | Use a dilute solution and a medium viscosity solvent like H2O. Analysis is best done using Topspin, not MNova. | projecteddosy_cc |
2Hzg (NEO400 and AV500 only) |
7min29s | 1D 2H, no decoupling. | Prepare sample in a protonated solvent! | zg2h |
7Li_ZG (NEO400 and AV500 only) |
12min6s | 1D 7Li, no decoupling. | zg | |
| B11ZG | 5min3s | 1D 11B, no decoupling. | zg | |
| B11_BS | 1min5s | 1D 11B, no decoupling. Background suppression. | zgbs | |
| B11_IGBS | 1min6s | 1D 11B, 1H decoupling during acquisition. Background suppression. | zgigbs | |
N14 (NEO400 only) |
6min8s | 1D 14N, no decoupling. | zg | |
| N15 | 6min30s | 1D 15N, no decoupling. | zg | |
| N15IG | 3min37s | 1D 15N, 1H decoupling during acquisition. | zgig | |
Mg25_zg (NEO400 only) |
1min5s | 1D 25Mg, no decoupling. | zg | |
Mg25_BS (NEO400 only) |
1min5s | 1D 25Mg, no decoupling. Background suppression. | zgbs | |
| AL27ND | 1min23s | 1D 27Al, no decoupling. | zg | |
SI29IG (NEO400 and AV500 only) |
13min22s | 1D 29Si, 1H decoupling during acquisition. | zgig | |
| SE77ZG | 1min43s | 1D 77Se, 1H decoupling during acquisition and a 30° pulse width for more accurate integrals. | zgig30 | |
SN119IG |
48s |
1D 119Sn, 1H decoupling during acquisition and a 30° pulse width for more accurate integrals. |
|
zgig30 |
__________________ |
_____________ |
_______________________________________ |
__________________________________ |
________________ |