synthesis and detection of oxygen-18 labeled phosphate合成的磷酸氧18标记和检测.pdfVIP

synthesis and detection of oxygen-18 labeled phosphate合成的磷酸氧18标记和检测.pdf

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synthesis and detection of oxygen-18 labeled phosphate合成的磷酸氧18标记和检测

Synthesis and Detection of Oxygen-18 Labeled Phosphate Eric S. Melby, Douglas J. Soldat*, Phillip Barak Department of Soil Science, University of Wisconsin-Madison, Madison, Wisconsin, United States of America Abstract Phosphorus (P) has only one stable isotope and therefore tracking P dynamics in ecosystems and inferring sources of P loading to water bodies have been difficult. Researchers have recently employed the natural abundance of the ratio of 18O/16O of phosphate to elucidate P dynamics. In addition, phosphate highly enriched in oxygen-18 also has potential to be an effective tool for tracking specific sources of P in the environment, but has so far been used sparingly, possibly due to unavailability of oxygen-18 labeled phosphate (OLP) and uncertainty in synthesis and detection. One objective of this research was to develop a simple procedure to synthesize highly enriched OLP. Synthesized OLP is made up of a collection of species that contain between zero and four oxygen-18 atoms and, as a result, the second objective of this research was to develop a method to detect and quantify each OLP species. OLP was synthesized by reacting either PCl5 or POCl3 with water enriched with 97 atom % oxygen-18 in ambient atmosphere under a fume hood. Unlike previous reports, we observed no loss of oxygen-18 enrichment during synthesis. Electrospray ionization mass spectrometertry (ESI-MS) was used to detect and quantify each species present in OLP. OLP synthesized from POCl contained 1.2% P18O16O , 18.2% P18O 16O , 67.7% 3 3 2 2 P18O 16O, and 12.9% P18O , and OLP synthesized from PCl contained 0.7% P16O , 9.3% P18O 16O, and 90.0% P18O . We 3 4

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