Preparation and evaluation of nickelmesogen for micropacked gas chromatography.
The preparation and mesomorphic properties of a substituted bis(dithiolene)nickel complex derived from 4, 4'-dimethoxybenzil are reported. The phase transition temperatures were based on data obtained by polarized light microscopy and differential scanning calorimetry. The mesogenic phase existed over the temperature range from 77 to 175 degrees C. A novel micropacked column (1.5 or 3 m x 1 mm i.d.) prepared from the slurry of bis[1,2-bis(4-n-undecyloxyphenyl)ethane-1,2-dithiolene] nickel(II) (5%, w/w), coated on Chromosorb W was applied for the separation of dialkyl sulfides. The non-linearity (discontinuity) of Van't Hoff plots suggests that the liquid crystal property existed even in the coated phase. Factors affecting the retention and the sample selectivity on the prepared column were examined by using a flame photometric detector (FPD). The separation might be based on the mechanism of ligand exchange, shape selectivity and polarity interaction besides the vapor pressure. LOD for the determination of dialkyl sulfides was below 1 ng for most of the analytes.
Chou
Chiann-Tyng
CT
Department of Chemistry, National Taiwan University, 1, Sec. 4, Taipei 10617, Taiwan.
Pai
Yi-Fen
YF
Lin
Chun-Chi
CC
Misra
Tarun K
TK
Liu
Chuen-Ying
CY
D002138:Calibration; D002849:Chromatography, Gas / Q000295:instrumentation* / Q000379:methods; D008024:Ligands; D009682:Magnetic Resonance Spectroscopy; D009532:Nickel / Q000737:chemistry*; D009942:Organometallic Compounds / Q000737:chemistry*; D012680:Sensitivity and Specificity; D013055:Spectrophotometry, Infrared
D008024:Ligands; D009942:Organometallic Compounds; D009532:Nickel