Techniques and Methods 10–C19
The purpose of the Reston Stable Isotope Laboratory lab code 1700 is to determine the δ2H/1H), abbreviated as δ2H, and the δ18O/16O), abbreviated as δ18O, of soil water and water in plant matter. This method is based on the observation that water and toluene form an azeotropic mixture at 84.1 °C. This temperature is substantially lower than the boiling points of water (100 °C) and toluene (110 °C), but water and toluene are immiscible at ambient temperature. The water content of a soil or plant is determined by weighing, drying, and reweighing a small amount of sample. Sufficient sample to collect 3 to 5 milliliters of water after distillation is loaded into a distillation flask. Sufficient toluene is added so that the sample is immersed throughout the entire distillation to minimize evaporation of water, which would affect the δ2H and δ18O values. The mixture of sample and toluene is heated in a flask to its boiling point (84.1 °C) so that water from the sample and toluene can distill together into a specially designed collection funnel. The temperature of 84.1 °C is maintained until the water has been quantitatively transferred to the collection funnel, at which time the temperature is raised to the boiling point of the remaining component (toluene, 110 °C). The collection funnel is maintained at ambient temperature so that the sample water and toluene can be separated physically. After separation, the sample water is purified by addition of paraffin wax to the container with the sample water, capping the container, and heating to approximately 60 °C to melt the wax. Trace amounts of toluene will dissolve in the wax, purifying the sample water for isotopic analysis.
The isotopic composition of the purified water is then determined by equilibration with gaseous hydrogen or carbon dioxide, followed by dual-inlet isotope-ratio mass spectrometry. Because laser-absorption spectrometry is sensitive to organic compounds, such as trace toluene remaining in water samples, water samples should be analyzed for isotopic composition only by mass spectrometry and not by laser-absorption spectrometry.
First posted July 30, 2012
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Révész, Kinga, Buck, Bryan, and Coplen, T.B., 2012, Determination of the δ2H and δ18O of soil water and water in plant matter; RSIL lab code 1700, chap. 19 of Stable isotope-ratio methods, sec. C of Révész, Kinga, and Coplen, T.B. eds., Methods of the Reston Stable Isotope Laboratory: U.S. Geological Survey Techniques and Methods, book 10, 21 p., available only at https://pubs.usgs.gov/tm/10c19/.
Summary of Procedure
Reporting Units and Operational Range
Reference Materials and Documentation
Labware, Instrumentation, and Reagents
Sample Collection, Preparation, Analysis, Retention Times, and Disposal
Data Acquisition, Processing, Evaluation, Quality Control, and Quality Assurance
Health, Safety, and Waste-Disposal Information
Appendix A. Example of a United States Department of Agriculture Permit to Receive Soil
Appendix B. Step-by-Step Procedure to Prepare and Analyze Samples for Distillation