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FP7

Certification of the Deuterium-to-Hydrogen (D/H) ratio in a 1,1,3,3-tetramethylurea Batch Certified Reference Material STA-003k

Funded under: FP7-JRC

Abstract

This report describes the production of a tetramethylurea reference material (STA-003k), certified for its deuterium-tohydrogen (D/H) amount-of-substance 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 amount-ofsubstance ratios of ethanol distilled from wines, an important measure in wine authenticity testing (Commission Regulation 2676/90, [1]).%:LCommercially obtained TMU with a sufficiently high D/H amount-of-substance ratio (> 120 x 10{-6}) was purified by removing most of the residual water and filled into amber glass bottles of 500 mL portions. Homogeneity was tested and no heterogeneity observed. Stability studies indicated no material degradation for 4 weeks at 60 ºC and a very minor degradation over a period of 5 years at 20 ºC which. Batch characterisation was accomplished in an inter-laboratory comparison using the SNIF-NMR 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.

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 23243 EN (2008), 38 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: 978-92-79-08346-4
Record Number: 200819702 / Last updated on: 2008-03-20
Category: PUBLICATION
Original language: en
Available languages: en