title: Preparation of hydrogen from water by reduction with lithium aluminium hydride for the analysis of delta(2)H by isotope ratio mass spectrometry.
abstract: An off-line technique is described for the preparation of H(2) from water prior to analysis of delta(2)H by dual-inlet isotope ratio mass spectrometry. H(2) is produced from sample water by reaction with LiAlH(4). This provides a rapid and inexpensive method for the analysis of delta(2)H in small (10 microL) samples of water. Precision was +/- 4.2 to 8.0 (1sigma(n), n = 8) delta(2)H(VSMOW) for samples between 428 and 1500 delta(2)H(VSMOW), +/- 14.5 delta(2)H(VSMOW) for water enriched to 3750 delta(2)H(VSMOW) and +/- 26.0 delta(2)H(VSMOW) for water enriched to 6100 delta(2)H(VSMOW). Accuracy was +/- 1.1 to 4.2 delta(2)H(VSMOW) for water standards from natural abundance to 1000 delta(2)H(VSMOW) (the highest enrichment at which water of accepted delta(2)H is currently available). This method for delta(2)H determination is most appropriate for use with small (<50 microL) samples of high delta(2)H enrichment such as those produced from doubly labelled water studies of small animals. The levels of measurement precision of delta(2)H would contribute 2.6-3.8% to the precision error in estimates of small animal energy expenditure made using the doubly labelled water technique when duplicate analyses are performed.
authors.affiliation: Aberdeen Centre for Energy Regulation and Obesity, Department of Zoology, University of Aberdeen, Tillydrone Avenue, Aberdeen AB24 2TZ, UK.
authors.forename: S
authors.initials: S
authors.lastname: Ward
authors.forename: M
authors.initials: M
authors.lastname: Scantlebury
authors.forename: E
authors.initials: E
authors.lastname: Król
authors.forename: P J
authors.initials: PJ
authors.lastname: Thomson
authors.forename: C
authors.initials: C
authors.lastname: Sparling
authors.forename: J R
authors.initials: JR
authors.lastname: Speakman
mesh_terms: D017607:Aluminum Compounds / Q000737:chemistry*; D003903:Deuterium; D006859:Hydrogen / Q000737:chemistry*; D018020:Lithium Compounds / Q000737:chemistry*; D013058:Mass Spectrometry; D010084:Oxidation-Reduction; D019163:Reducing Agents; D015203:Reproducibility of Results; D012623:Seawater / Q000032:analysis; D014867:Water / Q000737:chemistry*
chemical_list: D017607:Aluminum Compounds; D018020:Lithium Compounds; D019163:Reducing Agents; D014867:Water; C042073:lithium aluminum hydride; D006859:Hydrogen; D003903:Deuterium