nmr spectroscopy: preparing a samplechemh215/chem216/nmr/prep_nmrsample.… · web viewdilute the...
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NMR Spectroscopy: Preparing a Sample
Background ReadingDerome, A.E. Modern NMR techniques for chemistry research; Pergamon Press: Oxford, 1987.Harris, R.K. Nuclear Magnetic Resonance Spectroscopy; Longman: Essex, 1986. Hornak, J.P. Basics of NMR, http://www.cis.rit.edu/htbooks/nmr/, 2003.
Preparing a sampleFor the neat liquid compounds pipet 5-6 drops into a clean NMR tube. Dilute the sample with perdeuterated solvent until the solution fills approximately 3 cm of the NMR tube. For the solid organic compound place 10-15 mg of solid in a clean 1 dram glass vial and dissolve in a minimum of perdeuterated solvent. Transfer the solution to a clean NMR tube by pipet and fill the tube to a height of 3 cm with solvent. Place the plastic cap over the end of the NMR to prevent evaporation.
NOTE: IT IS VERY IMPORTANT TO AVOID CONTAMINATION OF THE CHEMICALS AND SOLVENTS USED IN THIS EXPERIMENT. NEVER PIPET DIRECTLY FROM A STOCK REAGENT BOTTLE!
Too little sample. Instrument will not lock
Too much sample. Instrument will not lock.
Waaaaay too much sample. Instrument will not lock.
Perfect amount of sample.