Approaches for the coating of capillary columns with highly phenylated stationary phases for high-temperature GC.

Two highly phenylated tetramethyl-p-silphenylene-diphenylsiloxane copolymers were coated on fused silica capillary columns and used as stationary phases in GC. The copolymers offered new insights into the coating process and column preparation due to their physicochemical properties. The fused silica capillary surface had to be pretreated in various ways to achieve a homogeneous film and a well deactivated surface: etching with ammonium bifluoride; leaching with sodium hydroxide and hydrochloric acid; silylation with tetraphenyldimethyldisilazane and triphenylsilylamine. Droplet formation was observed on tetraphenyldimethyldisilazane silylated surfaces leading to capillary columns with low separation efficiency. The topology of inhomogeneous films was investigated by light microscopy, scanning electron microscopy, and Auger electron spectroscopy. It became apparent that the stationary phase did not form droplets but islands, which are connected by a wetting layer according to the Stranski-Krastanov growth mode. Both copolymers are potential stationary phases for high-temperature GC with promising properties. They offer a higher overall polarity than 75% phenyl, 25% methyl-polysiloxanes in combination with increased thermal stability and reduced bleed levels.

[1]  H. Kählig,et al.  A 50% n-octylmethyl, 50% diphenyl-polysiloxane as stationary phase with unique selectivity for gas chromatography. , 2003, The Analyst.

[2]  H. Kählig,et al.  A trifluoropropyl‐containing silphenylene–siloxane terpolymer for high temperature gas chromatography , 2003 .

[3]  H. Kählig,et al.  Chromatographic properties of tetramethyl-p-silphenylene-dimethyl, diphenylsiloxane copolymers as stationary phases for gas-liquid chromatography. , 2003, Journal of chromatography. A.

[4]  J. Zeeuw,et al.  Use of novel stationary phases to reduce bleed by a factor of four , 2003 .

[5]  P. Zöllner,et al.  A new 75% diphenyl, 25% dimethyl‐polysiloxane coated on fused silica capillary columns for high temperature gas chromatography , 2002 .

[6]  H. Kählig,et al.  Characterization of stationary phases for gas chromatography by 29Si NMR spectroscopy. II. Silphenylene-siloxane copolymers. , 2001, Journal of chromatography. A.

[7]  Masa-aki Suzuki,et al.  Fabrication of Poly(diphenylsilylenemethylene) and Poly(diphenylsiloxane) Thin Films Using Fine Metal Particles , 1999 .

[8]  I. Mita,et al.  Mesomorphic behavior in polydiphenylsiloxane. 3. An examination of high molecular weight polydiphenylsiloxane , 1998 .

[9]  E. Lorbeer,et al.  Triacylglycerol mixture for testing capillary columns for high-temperature gas chromatography , 1997 .

[10]  E. Lorbeer,et al.  A fused silica capillary column coated with a medium polar stationary phase for HTGC , 1995 .

[11]  T. Welsch,et al.  The thermal immobilization of hydroxy-terminated silicone phases in high-temperature-silylated glass capillaries. A study of reaction mechanisms , 1991 .

[12]  H. Moser,et al.  Preparation of glass capillary columns with diphenyl phenylmethyl silicone (OV‐25) , 1986 .

[13]  W. Blum Preparation of glass capillary columns coated with immobilized OV‐240‐OH (33% cyanopropyl substituted, OH‐terminated). An approach to improve the inertness and thermal stability of cyanoalkyl polysiloxane coatings , 1986 .

[14]  J. Venables,et al.  Nucleation and growth of thin films , 1984 .

[15]  T. Nestrick,et al.  Etching borosilicate glass capillary columns , 1982 .

[16]  G. Guiochon,et al.  Capillary gas chromatography of azaarenes , 1982 .

[17]  B. W. Wright,et al.  The preparation of non-extractable methylphenylpolysiloxane stationary phases for capillary column gas chromatography , 1982 .

[18]  L. Blomberg,et al.  Preparation of capillary columns coated with phenylsilicone gum , 1982 .

[19]  B. W. Wright,et al.  Characterization of glass, quartz, and fused silica capillary column surfaces from contact-angle measurements , 1981 .

[20]  K. Grob,et al.  Deactivation of glass capillaries by persilylation. Part 3: Extending the wettability by bonding phenyl groups to the glass surface , 1980 .

[21]  M. P. Maskarinec,et al.  Surface Deactivation in Glass Capillary Columns and Its Investigation by Auger Electron Spectroscopy , 1979 .

[22]  K. Grob,et al.  Comprehensive, standardized quality test for glass capillary columns , 1978 .

[23]  T. Welsch,et al.  Zur Desaktivierung von Glaskapillaren mittels Silanisierung , 1977 .

[24]  M. Novotny,et al.  Surface chemistry of glass open tubular (capillary) columns used in gas-liquid chromatography , 1974 .

[25]  M. Donike Die temperaturprogrammierte Analyse von Fettsäuretrimethylsilylestern: Ein kritischer Qualitätstest für gas-chromatographische Trennsäulen , 1973 .

[26]  W. O. McReynolds,et al.  Characterization of Some Liquid Phases , 1970 .

[27]  L. Rohrschneider Eine methode zur chrakterisierung von gaschromatographischen trennflüssigkeiten , 1966 .