Thermally stable dexsil-400 glass capillary columns

Journal Article · Sat Mar 01 04:00:00 EST 1980 · Anal. Chem.; (United States)

DOI:https://doi.org/10.1021/ac50053a055· OSTI ID:5309691

Maskarinec, M P; Olerich, G

The factors affecting efficiency, thermal stability, and reproducibility of Dexsil-400 glass capillary columns for gas chromatography in general, and for polycyclic aromatic hydrocarbons (PAHs) in particular were investigated. Columns were drawn from Kimble KG-6 (soda-lime) glass or Kimox (borosilicate) glass. All silylation was carried out at 200/sup 0/C. Columns were coated according to the static method. Freshly prepared, degassed solutions of Dexsil-400 in pentane or methylene chloride were used. Thermal stability of the Dexsil 400 columns with respect to gas chromatography/mass spectrometry (GC/MS) were tested. Column-to-column variability is a function of each step in the fabrication of the columns. The degree of etching, extent of silylation, and stationary phase film thickness must be carefully controlled. The variability in two Dexsil-400 capillary column prepared by etching, silylation with solution of hexa methyl disilazone (HMDS), and static coating is shown and also indicates the excellent selectivity of Dexsil-400 for the separation of alkylated aromatic compounds. The wide temperature range of Dexsil-400 and the high efficiency of the capillary columns also allow the analysis of complex mixtures with minimal prefractionation. Direct injection of a coal liquefaction product is given. Analysis by GC/MS indicated the presence of parent PAHs, alkylated PAHs, nitrogen and sulfur heterocycles, and their alkylated derivatives. 4 figures. (DP)

• Research Organization: Oak Ridge National Lab., TN
• DOE Contract Number: W-7405-ENG-26
• OSTI ID: 5309691
• Journal Information: Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 52:3; ISSN ANCHA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102* -- Chemical & Spectral Procedures
AROMATICS
CHROMATOGRAPHY
ETCHING
EXTRACTION APPARATUSES
EXTRACTION COLUMNS
GAS CHROMATOGRAPHY
GLASS
HYDROCARBONS
MASS SPECTROSCOPY
ORGANIC COMPOUNDS
PHYSICAL PROPERTIES
POLYCYCLIC AROMATIC HYDROCARBONS
SEPARATION PROCESSES
SPECTROSCOPY
SURFACE FINISHING
THERMODYNAMIC PROPERTIES