Deuterium Oxide (D2O) Determination in Water by Gas Chromatography–Mass Spectrometry Following Deuterium Exchange Headspace Extraction

A reliable, simple and fast method for quantitative analysis of heavy water (D 2 O) was developed using deuterium exchange headspace extraction–gas chromatography–mass spectrometry. The method is based on incubating the acetic anhydride with D 2 O, CH 3 COOD formation, headspace extraction of CH 3 COOD (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 ( R 2 = 0.9998) in the concentration range of 1 × 10 3 –3 × 10 5 mg/L). This method can measure D 2 O concentrations in water from 0.27 g/L. It was applied for determination of D 2 O in distilled water with accuracy RSD ≤ 6% and precision RSD ≤ 4%.