Development of a sampling and analysis method for 4-vinyl-1-cyclohexene in air

Abstract

The purpose of this research was to develop an applicable sampling and analytical method to determine airborne 4-vinyl-1-cyclohexene concentrations which are usually found in the atmosphere of polybutadiene factories. A solid sorbent tube, containing two sections (100 mg in the front and 50 mg in the back) of activated coconut-shell charcoal was chosen for sampling 4-vinyl-1-cyclohexene vapor. The 4-vinyl-1-cyclohexene in the charcoal samples was desorbed with carbon disulfide and analyzed by gas chromatography equipped with a flame ionization detector. The suitable air flow rate, adsorption capacity, sample storage stability, desorption efficiency and reliability of the method for sampling and analysis of 4-vinyl-1-cyclohexene were evaluated. The method was applied to sampling and analysis of 4-vinyl-1-cyclohexene in the rubber industry. The results indicated a suitable air flow rate of 0.3 to 1.5 l/min. The adsorption capacity of 4-vinyl-1-cyclohexene on 100 mg of charcoal was 0.2134 mg. The 4-vinyl-1-cyclohexene adsorbed on the charcoal was stable for 7 d at room temperature or 21 d in a refrigerated condition. The average percent desorption efficiency of 4-vinyl-1-cyclohexene ranged from 90.45% to 97.04% with the loaded amount ranging from 0.412 to 8.250 μg using 1 ml carbon disulfide. The limit of detection of 4-vinyl-1-cyclohexene was 0.044 ng. The average percent recoveries (n=6) of 4-vinyl-1-cyclohexene adsorbed on charcoal ranging from 0.46 to 8.87 μg were 96.78-102.87% with relative standard deviations (RSDs) of 0.34-1.92%, respectively. The concentrations of 4-vinyl-1-cyclohexene ranged from 0.011 to 0.105 mg/m3 in the working environment of a polybutadiene factory.