Automated SPE and Fast GC-ECD Analysis of PCBs in Waste Oil

A fast SPE-GC-ECD method for the analysis of PCBs in waste oil was developed. A complete profi le was obtained following SPE with a 12 minute GC run-time using a modular accelerated column heater (MACH). Full automation of the sample preparation and analysis (except sample weigh-in) enables a daily throughput of 100 samples. A wide range of concentrations can be determined using a dedicated column and Electron Capture Detection (ECD). INTRODUCTION The offi cial method for the analysis of PCBs in waste oil (DIN EN 61619) is time consuming and labor intensive (dilutions; extraction, column preparation and cleaning; manual solid phase extraction...) and it requires a long GC run (around 40 min). Speed of analysis in capillary GC can be increased by using fast and ultra-fast temperature programming. In general, peak resolution will be reduced when the temperature gradient is very fast, but for several applications, some loss of resolution can be accepted. Recently, direct resistive heating of the capillary column resulting in very fast heating rates (> 1800 °C/min) has been introduced [1]. The system available via GERSTEL under the name Modular Accelarated Column Heater (MACH, GERSTEL GmbH, Mülheim an der Ruhr, Germany) is mounted onto the door of a standard GC holding up to four modules containing separate capillary columns