Abstract

This manual was devised as a one semester program of work for the Masters in Analytical Chemistry for one day per week. It was designed to demonstrate the analytical methodology and instrumentation utilized to proceed from the raw sample stage through sample preparation to the final analysis of reduced sample residues by capillary gas chromatography and GC/Mass Spectrometry. A variety of target analytes were employed to highlight the techniques to detect and quantify these compounds using external and internal standard addition, including selected priority pollutants , chloro-hydrocarbons (OCHs), polyaromatic hydrocarbons (PAHs) and chlorophenols. Liquid and solid matrices were employed to illustrate the analytical methodology, spiked with the target analytes to be monitored. The USEPA method 625 was adopted for liquid-liquid acid-base extraction of semi-volatile priority pollutants aimed at the demonstrating of quality assurance/control, recovery efficiency and application of derivatization to enhance detection. Solid phase extraction (SPE) of target analytes from water was utilized to illustrate the clean-up and concentration of analytes.Demonstration of on-column injection was illustrated for the profiling of n-alkanes and PAHs. The focus is the analytical methodology and procedures for presenting priority pollutant residues for analysis by GC-ECD and GC/EI or NICIMS. Representative data analyses, calibration and quantitation are not exemplified. Historic references relevant to the analytical methodology employed in the procedures for the laboratory manual are included.