A new and effective method for accurate water content determination using headspace gas chromatography/mass spectrometry (GC/MS) with the standard addition technique was developed. This method was applied to the analysis of commercially available water standards prepared in many kinds of solvent matrices. The results obtained were consistent with the standard specifications and the values obtained by Karl Fisher (KF) titration within the range of uncertainty. Furthermore, the method was also applied to biofuel samples such as biodiesel derived from palm. Finally, the results revealed that headspace GC/MS is a superior technique for water content analysis, and the developed method is applicable to a variety of analytes for which KF titration is not appropriate.
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