Abstract. Chemically bonded solid phase materials are very important in separation chemistry. The chemically modified silica gel contains rest silanol groups that can affect the retention properties when they are used for separation of compounds. Some commercially available solid phase extraction (SPE) materials based on silica gel were analysed for rest silanol groups by near infrared spectroscopy. The combination frequency of the water molecules in the 5500-5000 cm -1 region was used in identifying the nature of water molecules on the surface and the information was used to identify the types of silanol groups on the surface. Second derivative technique was employed in the detailed analysis.Nine different SPE materials including C18, C8, C 6 H 5 , NH 2 , OH, CN, SiOH, SA (SCX) and SB (SAX) were examined by near infrared spectroscopy for rest silanol groups. The results show that the non-polar and polar stationary phases contain vicinal silanol groups and the ion exchange solid phase materials contain free, vicinal and geminal silanol groups.
IntroductionSolid phase extraction (SPE) columns are important tools of an analytical chemist in pre-concentrating analyte from solutions containing the analyte. The separation is carried out by passing the solution containing the component of interest through a column containing a suitable SPE material. When suitable SPE material used, the separation is based on the fact that the solid phase has greater affinity to the solute or components a chemist wants to separate from the solution matrix. This fact helps a chemist to preconcentrate either analyte from a solution matrix (isolation) or get rid of unwanted components (interference retention) in the solution matrix so that the filtrate is free from interfering components in the determination of the analyte. When the retained components on the SPE material are of interest then the components are eluted from the stationary SPE material using a suitable eluent (elution). Solid phase extraction is very widely used in isolating the analyte of interest from a variety of samples such as urine, blood serum, water etc. The mechanism of interaction of the components in the solution matrix and the solid stationary phase includes non polar, polar interactions, van der Waals interactions etc.