An in situ drying method for preparing NMR samples with extremely low water content.
A very simple closed apparatus and procedure are described which allow in situ drying of NMR samples by using molecular sieves and the freeze-pump-thaw technique. Limitations of the method are discussed. With acetonitrile, a residual water content of 3 x 10(-4)M could be reached.
Goez
M
M
Fachbereich Chemie, Martin-Luther-Universität Halle-Wittenberg, Kurt-Mothes-Strasse 2, Halle/Saale, D-06120, Germany.
D000097:Acetonitriles / Q000494:pharmacology; D003890:Desiccation / Q000295:instrumentation / Q000379:methods*; D005240:Feasibility Studies; D005612:Freeze Drying / Q000295:instrumentation / Q000379:methods; D009682:Magnetic Resonance Spectroscopy; D012996:Solutions / Q000737:chemistry*; D012997:Solvents / Q000737:chemistry*; D014867:Water / Q000032:analysis*
D000097:Acetonitriles; D012996:Solutions; D012997:Solvents; D014867:Water; C032159:acetonitrile