High accuracy isotope dilution analysis for the determination of ethanol using gas chromatography-combustion-isotope ratio mass spectrometry

Abstract

A procedure was established for the determination of ethanol in water samples by isotope dilution analysis. After spiking the sample with labelled [13C2]ethanol, it was analysed by gas chromatography-combustion-isotope ratio mass spectrometry. Results are reported for two certified reference materials and also ethanol solutions prepared for a CITAC (Co-operation on International Traceability in Analytical Chemistry) interlaboratory comparison. The certified reference materials were certified using the dichromate titration method at nominal levels of 80 and 200 mg per 100 mL. The CITAC solutions were prepared gravimetrically at nominal levels of 50, 80 and 200 mg per 100 mL. The results of the analysis agree well to within 0.5% of the gravimetric values of the different samples. The relative expanded standard uncertainties (with a coverage factor equal to 2) associated with the results varied between 0.18 and 0.37%, a range that encompassed the gravimetric values for the different samples. A complete uncertainty budget was also drawn up so that the different contributions could be identified and quantified. The main contributions were due to variations in the measured isotope amount ratios and a 'between' blend component introduced to quantify the contribution of factors such as the degree of matching of the isotope amount ratios between standards and samples used in the isotope dilution analysis.