Calibration of isotope ratio mass spectrometry working standard for 2H/1H ratio analysis

• Published in: Journal of mass spectrometry. Vol. 33; no. 7; pp. 627 - 630
• Main Authors: Lee, W.-N. Paul, Lim, Shu, Bassilian, Sara, Bergner, E. Anne
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01.07.1998; Wiley
• Subjects: 2H/1H ratio; Analytical biochemistry: general aspects, technics, instrumentation; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Calibration; Deuterium - analysis; Deuterium Oxide - chemistry; Fundamental and applied biological sciences. Psychology; Hydrogen - analysis; Isotope Labeling; isotope ratio mass spectrometry; Mass Spectrometry - methods; Mass Spectrometry - standards; Water - chemistry; working standard; Deuterium; Isotopic analysis; Calibration; Hydrogen Isotopes; Mass spectrometry
• ISSN: 1076-5174; 1096-9888
• DOI: 10.1002/(SICI)1096-9888(199807)33:7<627::AID-JMS677>3.0.CO;2-7

A method is described for the calibration of an isotope ratio mass spectrometry working standard for 2H/1H analysis using highly purified (>99.99% enriched) deuterium oxide (2H2O). Serial dilution of such a compound can be used to construct a standard curve for calibration purposes using the relationship APE/100=δD(SA)WR‐δD(BKG)WR1000×rWR . where APE is the atom percent excess. It was found that the determined rWR had a precision of ±1%. Most of the variation came from sample handling, which includes the serial dilution of the weighed deuterium oxide, the reduction of water to hydrogen gas and the introduction of the hydrogen gas into the mass spectrometer. The use of this calibration procedure allows the direct determination of the isotope ratio rSA, and APE from a standard curve over a wide range of enrichment. Unlike the reference standards V‐SMOW and SLAP, the highly purified deuterium oxide is non‐exhaustible and readily available. The highly purified deuterium oxide should be used in place of secondary standards to calibrate working references for 2H/1H analysis in biological studies. © 1998 John Wiley & Sons, Ltd.