CHNSO Elemental Analyses of Volatile Organic Liquids by Combined GC/MS and GC/Flame Ionisation Detection Techniques with Application to Hydrocarbon-Rich Biofuels

Elemental analysis is a fundamental method for determining the carbon, hydrogen, nitrogen, sulphur, and oxygen (CHNSO) contents in organic materials. Automated conventional elemental analysers are commonly used for CHNSO determinations, but they face challenges when analysing volatile organic liquids due to sample losses. This present study explores the combination of gas chromatography–mass spectrometry (GC/MS) and gas chromatography–flame ionisation detection (GC/FID) as a more accurate alternative method for elemental analysis of such liquids. Six different liquid samples containing various organic compounds have been analysed using both a conventional elemental analyser (Method 1) and the combined GC/MS–GC/FID method (Method 2). The results showed that Method 1 gave results with significant errors for carbon (by more than ±10 wt%) and oxygen (by up to ±30 wt%) contents due to volatile losses leading to inaccurate “oxygen-by-difference” determinations. In contrast, Method 2 gave more accurate and consistently representative elemental data in a set of simulated samples when compared to theoretical elemental data. This work proposes the use of the GC/FID method as a reliable alternative for CHNSO analysis of volatile organic liquids and suggests that employing the GC/FID technique can mitigate the common errors associated with conventional CHNSO analysis of such samples. However, successfully using Method 2 would depend on the skills and experience of users in qualitative and quantitative organic chemical analyses by gas chromatography.