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[Refining sample preparation procedures for solution 3P-NMR analysis of organic P in sediment]
Xiu-Ling Bai1, Yun-Kai Zhou, Bin Li
1Institute of Natural Resources and Environment, Henan University, Kaifeng 475004, China. bxling@163.com
Abstract:
Solution phosphorus-31 nuclear magnetic resonance spectroscopy (31P-NMR) is a novel technology in characterization of organic phosphorus (P) composition in sediments. This study was aim to refine sample preparation procedures for 31P-NMR, including determination of sample pretreatment, extraction time, sample to extractant ratio and concentration method. The results showed that recovery of P with air dried sample treatment was higher than that for the fresh samples. Most of the P was extracted within the first 8 hours, and the time could extend to 12 to 16 hours in order to improve the recovery of P. Using the extraction ratio [m(sediment): V(extractant)] of 1:8 received more spectral signals compared to 1:20 when both the extracts were concentrated at the same time. No evident loss of P was found when the extract was concentrated at 28 degrees C followed by centrifugation under low temperature.
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