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FP7

Certification of the Deuterium-to-Hydrogen (D/H) ratio in a 1,1,3,3-tetramethylurea master batch IRMM-425

Funded under: FP7-JRC

Abstract

This report describes the production of a tetramethylurea reference material (IRMM-425), certified for its deuterium-to-hydrogen (D/H) ratio. The material is to be used as an internal standard in site-specific natural isotope fractionation - nuclear magnetic resonance (SNIF-NMR) spectroscopy measurements for determining the D/H ratios of ethanol distilled from wines, an important measure in wine authenticity testing (Commission Regulation 2676/90, [1]).
Commercially obtained TMU with a sufficiently high D/H ratio (>120 x 10{-6}) was purified by removing most of the residual water and filled into amber glass ampoules in 7.8 mL portions. Homogeneity was tested and no heterogeneity observed. Stability studies indicated no material degradation for 4 weeks at 60 ºC and for 18 months at -20 ºC. Batch characterisation was accomplished in an inter-laboratory comparison using the SNIFNMR technique exclusively.
The certified value was obtained as the unweighted mean of the laboratory means of the accepted sets of results. The expanded uncertainty associated (k = 2) includes contributions from (potential) heterogeneity, potential instability, characterisation, as well as the carried-over uncertainty from BCR-656 (96% wine ethanol) that was used as the internal standard in the measurements. Due to its negligible contribution, the uncertainty associated with the purity of the material did not need to be included.

Additional information

Authors: ZELENY R, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);EMTEBORG H, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE);ULBERTH F, European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Geel (BE)
Bibliographic Reference: EUR 23031 EN (2007), 37 pp. Free of charge
Availability: Available from European Commission, JRC Knowledge Management Unit, Ispra (IT) Tel: +39 033278 9893 Fax: +39 033278 5409 E-mail: jrc-info@ec.europa.eu or Bruxelles (BE) Tel: +32 2 295 76 24 Fax: +32 2 299 63 22
ISBN: ISBN: 978-92-79-07550-6
Record Number: 200819704 / Last updated on: 2008-03-20
Category: PUBLICATION
Original language: en
Available languages: en