Abstract

A reliable, simple and fast method for quantitative analysis of heavy water (D2O) was developed using deuterium exchange headspace extraction–gas chromatography–mass spectrometry. The method is based on incubating the acetic anhydride with D2O, CH3COOD formation, headspace extraction of CH3COOD (exchange of hydrogen for deuterium) and gas chromatography/mass spectrometry detection. The quantification was performed using single ion monitoring (m/z = 61). The calibration was linear (R2 = 0.9998) in the concentration range of 1 × 103–3 × 105 mg/L). This method can measure D2O concentrations in water from 0.27 g/L. It was applied for determination of D2O in distilled water with accuracy RSD ≤ 6% and precision RSD ≤ 4%.

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