8. Overview of the most important VNMRJ parameters
There are well over a hundred parameters in VNMR. Some are of very little importance to the routine user. Only acquisition parameters are listed in the sequence as they appear in the parameter window and/or in a parameter printouts.
8.1 1D Data acquisition (i300, i400, s400, m400, ibd5, u500, i600)
parameter |
typical values |
explanation |
ACQUISITION |
||
sfrq [MHz] |
i300: 299.961 i|m400: 399.798 u500: 499.849 i600: 599.932 |
spectrometer frequency
basic Larmor frequency, depends on spectrometer; cannot be set by user |
tn | H1 C13, N15, P31 |
transmitter nucleus
always H1 on i300 and i600; other nuclei possible on i400, m400, ibd5 and u500 |
at [sec] |
1D: 2.0 or more 2D: 0.2 to 0.8 |
acquisition time
length of FID;
determines
digital
resolution: note: at = np/(2*sw) |
np [points] |
i300: 14,400 i|m400: 19,200 u500: 24,000 i600: 28,800 |
number of data points more needed at higher fields to maintain digital resolution note: at = np/(2*sw) |
sw [Hz] |
i300: 3600 i|m400: 4800 u500: 6000 i600: 7200 |
sweep width more needed at higher fields to cover 12 ppm range note: at = np/(2*sw) |
fb [Hz} |
not used | filter bandwidth
often replaced by DSP, therefore not used |
bs | 4-8 | block size
number of transients after which data are sent from the console to the host computer |
ss | 2-4 | steady-state pulses (also known as dummy scans)
number of complete executions of the pulse sequence prior to actual data collection |
tpwr [dB] |
59 (or less), other values common for special techniques |
transmitter power
level Note: for every 6 dB down, pw doubles |
pw [msec] |
5 to 15 | pulse width
length of a radio frequency pulse to rotate magnetization from z to xy-plane; depends on probe, tpwr, spectrometer |
p1 [msec] |
0 | length of
additional pulse(s) in the sequence
often not used |
d1 [sec] |
3.0 in 1D 0.8 to 1.2 in 2D |
1st
delay relaxation time; allowing the magnetization to return to the z direction |
tof [Hz] |
transmitter offset solvent and field dependent |
|
gain [dB] |
16-32 | receiver gain sensitivity of the receiver; too high causes ADC overflow and serious baseline distortions Note: for every 6 dB increase, the sensitivity doubles |
nt | 1, 2, 3,
4
4, 8, 16, 32, 64 |
number of transients signal-to-noise increases with ; usually multiples of 4 or 8 required except for gradient-enhanced techniques where any integer is possible; for indefinite acquisition (runs until stopped by aa) enter 1e9 |
ct | -- |
completed transients cannot be changed by user; if exp. runs to completion then ct = nt |
seqfil | s2pul, aogcosy, gHMQC . | name of the
pulse sequence's file name s2pul is used for standard 1D spectra |
SAMPLE |
||
date | -- | date the
spectrum is recorded (not processed) entered automatically by the system |
solvent | d2o, cdcl3, cd3od, cd2cl2 | lock solvent directly affects tof and referencing of spectrum; read in with parameter sets and should not be changed unless solvent is not in the list D2O and d2o etc. are identical (only for this parameter; this is an exception under UNIX!) |
file | exp or real filename |
file name of
parameter set or data file reads exp when an experiment is complete; when data are saved and read back, file shows the full name including the path |
DECOUPLING |
||
dn | H1, C13, N15 |
decoupler nucleus
H1 for homonuclear exp. |
dof [Hz] |
decoupler offset for solvent presaturation set to solvent resonance; for heteronuclear decoupling set to middle of frequency range of decoupled nucleus; both depends on the field and the solvent (i.e. the lock frequency) |
|
dm | nnn, ynn, nny | decoupler mode pulse sequences are divided into several time intervals (many have 3) and each letter defines whether the decoupler is on (at frequency dof and power dpwr) or off in the respective time interval n for no decoupling, y turns the decoupler on |
dmm | c, w, g |
decoupler modulation mode for presaturation of solvent c; for broadband decoupling of entire nucleus w (WALTZ) or g (GARP) |
dmf |
decoupler modulation frequency inactive for dmm=c |
|
dpwr [dB] |
-16 to 45 |
decoupler power
level controls the power level of the decoupler channel; depends on solvent (for presaturation) and band width for heteronuclear broadband decoupling which is a function of the field strength Note: for every 6 dB up, the power doubles |
homo | y or n |
homodecoupling control y for homonuclear decoupling, n for heteronuclear decoupling, both require y in the correct place of dm to turn the decoupler actually on |