Gas Chromatographic Detection of Tris(2-chloroethyl) and Tris(2-butoxyethyl)phosphate in Groundwater by Large-Sample-Volume Injection

Abstract

Abstract A capillary gas chromatograph equipped with a flame photometric detector (GC–FPD) for splitless injection of large sample volume was developed. The GC–FPD effectively diverted dichloromethane from the analytical column through a solvent diversion column and quantitatively retained tri(2-chloroethyl) phosphate (TCEP) and tris(2-butoxyethyl)- phosphate (TBXP) on a cold-trap column in front of the analytical column. The optimum conditions for 100 uL injections of TCEP and TBXP in dichloromethane at concentrations from 1 to 100 ng/mL were investigated. With the GC–FPD, relative standard deviations of the peak area and the retention time of the triesters injected at 10 ng/mL were less than 7.0 and 0.05%, respectively. These results were similar to those from normal splitless injection of 1 μL at 1 μg/mL in dichloromethane. A screening method for TCEP and TBXP in groundwater combined with liquid–liquid extraction with dichloromethane permitted detection at low nanogram-per-liter levels. Recoveries of TCEP and TBXP in 500 mL of groundwater were greater than 77.2 and 81.4%, respectively, each at fortified level of 10ng/L.