NMR Spectroscopy: Preparing a Samplechemh215/CHEM216/NMR/prep_nmrsample.… · Web viewDilute the...
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NMR Spectroscopy: Preparing a Sample Background Reading Derome, 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 sample For 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.
Transcript of NMR Spectroscopy: Preparing a Samplechemh215/CHEM216/NMR/prep_nmrsample.… · Web viewDilute the...
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.
