nmr spectroscopy: preparing a samplechemh215/chem216/nmr/prep_nmrsample.… · web viewdilute the...

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.

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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.

http://www.cis.rit.edu/htbooks/nmr/

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