Method Validation for Analysis of Aroclor 1260 in Transformer Oil using Gas Chromatography – Electron Capture Detection

Abstract

Since early 1980’s, the production and usage of Polychlorinated biphenyls (PCBs) have been banned throughout the world due to its carcinogenicity to humans and animals. However, due to the large half-lives of PCBs, large amounts of stocks are still available in storage. This study presents the validation data of the method developed for analysis of Aroclor 1260 in transformer oils in order to determine the concentrations for systematic disposal and destruction. The transformer oil samples were prepared according to the ASTM D 4059 with few modifications. PCBs in transformer oils were extracted with iso-octane followed by deactivated florisil cleanup and detection by GC – ECD using HP 5 GC column (30 m x 0.32 mm x 0.25 μm). The study was performed under matrix matched condition to eliminate the matrix effect that was found to be significant. The method was found linear over a wide working range from 2.5 ppm – 100 ppm with a regression coefficient of 0.994 and a lower limit of determination of 2.5 ppm. Method showed satisfactory repeatability with relative standard deviation below 7% over the entire working range. Accuracy of the method was assured using spike recoveries at 5 ppm, 10 ppm and 50 ppm with 85%, 105% and 93% respectively. The selectivity of Aroclor 1260 was confirmed against Aroclor 1254 and Aroclor 1242 considering uniquely identified non – overlapping chromatographic peaks. Based on the performance characteristics, this method can be suggested as an accurate and precise methodology to analyze Aroclor 1260 present in transformer oil.