Preparation of hydrogen from water by reduction with lithium aluminium hydride for the analysis of δ2H by isotope ratio mass spectrometry
✍ Scribed by Sally Ward; Michael Scantlebury; Ela Król; Peter J. Thomson; Carole Sparling; John R. Speakman
- Publisher
- John Wiley and Sons
- Year
- 2000
- Tongue
- English
- Weight
- 53 KB
- Volume
- 14
- Category
- Article
- ISSN
- 0951-4198
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✦ Synopsis
An off-line technique is described for the preparation of H 2 from water prior to analysis of d 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 d 2 H in small (10 mL) samples of water. Precision was AE 4.2 to 8.0 (1' n , n = 8) d 2 H VSMOW for samples between 428 and 1500 d 2 H VSMOW , AE 14.5 d 2 H VSMOW for water enriched to 3750 d 2 H VSMOW and AE 26.0 d 2 H VSMOW for water enriched to 6100 d 2 H VSMOW . Accuracy was AE 1.1 to 4.2 d 2 H VSMOW for water standards from natural abundance to 1000 d 2 H VSMOW (the highest enrichment at which water of accepted d 2 H is currently available). This method for d 2 H determination is most appropriate for use with small (`50 mL) samples of high d 2 H enrichment such as those produced from doubly labelled water studies of small animals. The levels of measurement precision of d 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.