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We present a new set of reference materials, the ND70‐series, forin situmeasurement of volatile elements (H₂O, CO₂, S, Cl, F) in silicate glass of basaltic composition. The materials were synthesised in piston cylinders at pressures of 1 to 1.5 GPa under volatile‐undersaturated conditions. They span mass fractions from 0 to 6%m/mH₂O, from 0 to 1.6%m/mCO₂and from 0 to 1%m/mS, Cl and F. The materials were characterised by elastic recoil detection analysis for H₂O, by nuclear reaction analysis for CO₂, by elemental analyser for CO₂, by Fourier transform infrared spectroscopy for H₂O and CO₂, by secondary ion mass spectrometry for H₂O, CO₂, S, Cl and F, and by electron probe microanalysis for CO₂, S, Cl and major elements. Comparison between expected and measured volatile amounts across techniques and institutions is excellent. It was found however that SIMS measurements of CO₂mass fractions using either Cs⁺or O⁻primary beams are strongly affected by the glass H₂O content. Reference materials have been made available to users at ion probe facilities in the US, Europe and Japan. Remaining reference materials are preserved at the Smithsonian National Museum of Natural History where they are freely available on loan to any researcher.