#Inmr from scan pdf#

I) since natural linewidths are 5-10 times wider than in 1H spectra, viscosity is usually not a factor. deuterated DMSO, benzene, pyridine, H2O, etc.)įor 13C spectra concentrations of 10-300 mgs/0.4 ml are common depending on MW. Iii) high viscosity solvents should be avoided if really sharp spectra are desired (e.g. Ii) chemical shift (δ) can vary due to solvent, or temperature, or concentration. I) dilute solution is better than concentrated since linewidth (Δ1/2) increases with increasing viscosity. Concentration: For 1H spectra (high resolution Δ1/2 < 0.5 Hz) generally used <1 to ~40 mgs/0.4 ml depending on molecular weight. If sample volume is significantly different (larger or smaller from the optimum 4.5 cm depth) then either longer SHIMMING or GRADSHIMMING will be required to get good resolution, especially for proton spectra.Ĥ. If you are using larger volume (> 4.5 cm), do not center your solution, place NMR tube in spinner to a depth of 20 mm from the centre of coil. In this case you need to optimize position of the tube in the spinner turbine by centering volume of your sample relative to the centre marker on the depth gauge. If you are limited by quantities of sample, submit sample for AV600 or you can use lower volume (~ 3.0 cm) of solution on other spectrometers. Sample volume: 4.5 cm of solution should be used for different probes on AC200, AV300, AV400, AM400 magnets exactly 4.0 cm of solution required for the cryoprobe on AV600. Solvent: Choice of the solvent depends on the solubility of your sample, chemical shift of the residual protons in 1H NMR and position of signals in 13C NMR (position of the solvent peaks can overlap with signals from your compound), chemical (solvent should be inert towards your compound) and physical (b.p., m.p., viscosity need to be considered while doing VT NMR experiments) properties of the solvent.ģ. If you are using base bath for cleaning, make sure that you remove all traces of base by washing with acidic solution, water and acetone. Scratching tubes should be avoided (use copper wire in case of absolute needs). Usually J-Young tubes with larger valves give more problems during locking/shimming, which result in poor resolution.Ĭleaning NMR tubes could be done by rinsing with appropriate solvent. While you are choosing J-Young tube, be aware, that size of the valve does matter for our current setup (using string for lifting such tubes). If you are using repaired J-Young tube, make sure the sealing is as good as possible. The J-Young NMR tubes had to be at least 14 cm long before the valve. The “standard” NMR tubes had to be at least 15 cm long. High precision 5 mm NMR tubes should be used for AV600 cryoprobe and for high quality spectrum on AV400inv/dir. We are using 5 mm NMR tubes for all our spectrometers. NMR tubes: Quality has to comply with requirement for your NMR experiment. While preparing your NMR sample, please, pay attention to the following:ġ. Preparation of the NMR samples has to be done in your own work space.We do not have facilities (fume hood, selection of the solvents, NMR tubes etc.) to do this in the NMR laboratory. and print a hard copy, or we can send your raw data via e-mail as a zipped file and you can process it on your own computer using XWIN-NMR or Mest-Rec, or other available software. Your sample will be done on a “first come - first served” basis.

In order to submit sample for the service, please bring prepared sample in NMR tube to room B460, and fill the requisition form. For exceptional needs we have limited ability to run experiments on AV600 as well - please discuss your experiments with NMR staff. We offer technician based service on AV400inv/dir.

#Inmr from scan pdf#

Spectrometer time reservation policies: General Booking Policiess in the NMR LabĪll spectrometers combined in one PDF file