NMR Facility - Chemistry Department

Experiments for Automation

Parameter sets available on automated instruments

Experiments Available in Automation
(400-1 & new 400-2)

Experiment times do not include overhead for sample changing, tuning, locking, shimming, or setting gain.

Parameter Set

Default Time

Description

Pulse Sequence

PROTON1 20 sec 1D 1H, single scan with 90° excitation, 17 sec delay to allow for full relaxation. zg
PROTON8 36 sec 1D 1H, 8 scans, optimized for maximum signal and reliable integrals. For all multi-scan 1H 1D spectra with more scans, use these parameters and change NS.
See blog post for optimization details
zg30
CARBON 10 min 1D 13C, 128 scans. Provides OK S/N for 10 mg samples. Change NS, but not D1, AQ, or P1, for increased signal.
See blog post for optimization details
zgdc30
CARBON_3.5hr 3.5 hr Same as CARBON, but with NS=4096.
Night queue only
zgdc30
DEPT135 2 min 1D 13C DEPT135. 13C-detected, but signal enhanced via 1H magnetization. Only 13C atoms with 1H’s attached are observed. When properly phased, CH and CH3 13C’s are positive, CH2’s are negative. deptsp135
COSY-opt 8.5 min 2D COSY (COrrelation SpetroscopY), Indirect TD fixed at 200 increments. cosygpppqf
HSQC-opt 10 min 2D 1H-13C HSQC (Heteronuclear Single Quantum Coherence), indirect TD fixed at 128 increments; multiplicity-edited so CH and CH3 peaks are positive and CH2 are negative (as in a DEPT135 spectrum), sensitivity improved over standard. Gives very good signal levels on samples less than 10 mg. hsqcedetgpsisp2.4
HMBC-opt 22 min  2D 1H-13C HMBC (Heteronuclear Multiple Bond Correlation), indirect TD fixed at 256 increments, filters eliminate one-bond correlations. Gives good signal on 10 mg samples. hmbcetgpl3nd
NOESY-opt 2.25 hr 2D NOESY (Nuclear Overhauser Effect SpectroscopY) for detecting/measuring 1H-1H through-space contacts and chemical exchange, indirect TD fixed at 256 increments, default mixing time D9 = 0.6 sec (but can be modified). Sophisticated pulse sequence elements reduce DQCOSY-like +/- zero-quantum coherence (ZQC) artifacts. With positive diagonal peaks, negative crosspeaks indicate NOE and/or chemical exchange. Gives good data on 10 mg samples in the time specified.
Night queue only.
noesygpphzs
ROESY-opt 52 min 2D ROESY (ROtating frame noESY) for detecting/measuring 1H-1H through-space contacts and chemical exchange leveraging rotating-frame magnetization, indirect TD fixed at 128 increments, default mixing time is 0.6 sec. Also known as the “EASY-ROESY”, this “jump-symmetrized” ROESY reduces TOCSY artifacts and improves sensitivity. With positive diagonal peaks, positive crosspeaks indicate NOE contacts, and negative crosspeaks indicate chemical exchange. Gives good data on 10 mg samples in the time specified.
Night queue only.
roesyadjsph
TOCSY-opt 42 min 2D 1H-1H TOtal COrrelation SpectroscopY with DIPSI spin lock for detecting peaks in the same network of 1H-1H coupled spins, indirect TD fixed at 128 increments, default mixing time D9 = 0.08 sec that can be changed by user. dipsi2gpphzs
HSQC-TOCSY-opt 15 min 2D 1H-13C correlation combined with TOCSY; with 1H direct detection axis, 13C indirect detection. Each 13C resonance is coupled to the 1H covalently attached AND the 1H resonances in its 1H-1H spin-coupled network; excellent for assigning 1H peaks overlapped in 1H, COSY, and TOCSY spectra. Indirect TD fixed at 200 increments, default mixing time D9 = 0.045 sec. hsqcdietgpsisp.2
CHARACTERIZATION 55 min Sets up PROTON8, CARBON, DEPT135,COSY,HSQC,HMBC in one click various
FLUORINE 3 min 1D 19F with 90° excitation and 1H decoupling during acquisition. Uses a special spin-echo pulse sequence to eliminate background 19F signals from Teflon.
See blog post for optimization details.
zgfhigqn.2_se.jk
FLUORINE90 3 min 1D 19F with 90° excitation and no 1H decoupling or background-reducing pulse sequence. zg
PHOSPHORUS30 1 min 1D 31P with 30° excitation and no 1H decoupling zg30
PHOSPHORUS30_1Hdec 1 min 1D 31P with 30° excitation and 1H decoupling. zgig30
std11B.SMP 1 sec* 1D 11B with 90° excitation and no 1H decoupling, *NS=1 scan by default zg
LITHIUM7_3min 3 min 1D 7Li with 30° excitation and no 1H decoupling zg
HN-HSQC-opt 11 min 2D 1H-15N HSQC with indirect TD = 200 increments. Gives OK spectra on 10 mg samples
HN-HMBC 40 min 2D 1H-15N HMBC with indirect TD = 256 increments. Gives good spectra on 10 mg samples.
Night queue only.
PROTON_T1 2 hr Pseudo-2D T1 measurement experiment with 16 time points. For processing instructions, click here to access Bruker’s Advanced 1D and 2D Experiments guide.
Night queue only.
t1ir

 

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