NMR样品管.doc

How to make an NMR sample Safety warning: Some of the procedures described here are potentially dangerous. If you are unfamiliar with laboratory safety, please ask a qualified chemist for help. Samples for full service should be sufficiently soluble in the solvent requested. If not submitting for full service then please prepare your samples as follows. NMR tubes Samples for NMR analysis should be submitted in 5 mm NMR tubes [In cases of low solubility or low sensitivity for 13Carbon, 15Nitrogen, 31Phosophorus and 7Lithium NMR it may be desirable to submit samples in 10 mm NMR tubes for 400 MHz analysis. Samples for (39K) potassium and (183W) tungsten NMR may be submitted in 10 mm tubes for 300 MHz analysis.] Select the right type of NMR tube. For 300 MHz NMR tubes of the quality of Wilmad 507-PP-7, Aldrich series 300 or Kontes grade 3 are sufficient. For 400 MHz NMR use Willmad 528-PP-7, Aldrich series 400 or Kontes grade 6. (For 11B NMR use 528-PP-QTZ. For 10 mm tubes use 513-PP.) If the sample dissolves glass (e.g. HF) use a PTFE insert. Please label your tubes clearly with an appropriate concentric label. Examples of incorrect and correct NMR tube labels Solvent We do not have the equipment for solid state NMR so samples must be submitted in solution. Solvent selection is dictated by a number of factors. 1) It is general practice to use deuterated solvents for two reasons. a) The deuterium can be used for field frequency lock, making spectral resolution easier to assure and thereby saving you valuable service time. b) Solvents containing regular hydrogen yield large signals that may swamp those of your sample: the situation is made worse by saturation effects that broaden large signals. We recommend the use of deuterated solvents wherever possible. 2) The sample must be sufficiently soluble to yield an NMR spectrum. For 1H and 1H observed NMR, it is recommended to dissolve between 2 and 10 mg in between 0.6 and 1 mL of solvent so that the sample depth is at