This paper reports the development of an easy, fast and effective procedure for the verification of the ideal gas law in splitless injection systems in order to improve the response. Results of a group of pesticides were used to demonstrate the suitability of the approach. The procedure helps establish experimental parameters through theoretical aspects. The improved instrumental response allowed extraction with lower sample volumes, the minimization of time and costs and the simplification of sample preparation.

A simple chemical method has been developed to quantify the silanol groups (º Si-OH) in silica as well as in coated chromatographic supports for use in packed - column Gas Chromatography. After adsorption of 10 mg/mL methylene blue, centrifuging action and filtration, the absorbance of the solution was inversely proportional to the silanol quantity. The difference between the absorbance of the pure solution and that of the solid - free filtrate was related to the silica weight, yielding a quantitative analysis of these groups.

A imobilização de uma fase estacionária de silicone (SE-30) sobre Chromosorb W-AW para uso em cromatografia gasosa foi iniciada por peróxido de dicumila (DCUP). Foram estudadas concentrações apropriadas de peróxido e o procedimento utilizado para imobilização é bem descrito. Foram realizados testes de extrações com solventes, avaliação cromatográfica, bem como estabilidade térmica e lavagem com solventes em coluna. Estes testes mostraram que a preparação de SE-30 imobilizada sobre Chromosorb W-AW, usando DCUP, é simples e produz fases estacionárias eficientes e resistentes a solventes.

The immobilization of a silicone stationary phase (SE-30) on Chromosorb W/AW for use in packed column gas chromatography was initiated by dicumyl peroxide (DCUP). Appropriate peroxide concentrations were studied and the immobilization procedure is described. Solvent extractions and chromatographic testing, as well as thermal stability and on-column solvent rinsing, showed that preparation of an SE-30 phase immobilized on Chromosorb W/AW using DCUP is a simple method that produces efficient and non-extractable stationary phases.