Improved 31 P NMR analysis of phosphorus in highly mineralized lake water using a modified pretreatment procedure with H resin.

Chemosphere(2023)

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摘要
P Nuclear Magnetic Resonance (P NMR) is an important analytical tool for identifying and quantifying phosphorus-based compounds in aquatic environments. However, the precipitation method typically used for analyzing phosphorus species via P NMR has limited application. To expand the scope of the method and apply it to highly mineralized rivers and lakes worldwide, we present an optimization technique that employs H resin to assist phosphorus (P) enrichment in highly mineralized lake water. To explore how to reduce analysis interference from salt in highly mineralized water and improve the accuracy of P analysis using P NMR, we conducted case studies on Lake Hulun and Qing River. This study aimed to increase the efficiency of phosphorus extraction in highly mineralized water samples by using H resin and optimizing key parameters. The optimization procedure included determining the enriched water volume, H resin treatment time, AlCl addition amount, and precipitation time. The final recommended optimization enrichment procedure involves treating 10 L of filtered water sample with 150 g of Milli-Q water-washed H resin for 30 s, adjusting the pH of the treated sample to 6-7, adding 1.6 g of AlCl, stirring the mixture, and allowing the solution to settle for 9 h to collect the flocculated precipitate. The precipitate was then extracted with 30 mL of 1 M NaOH +0.05 M DETA extraction solution at 25 °C for 16 h, and the supernatant was separated and lyophilized. The lyophilized sample was redissolved in 1 mL of 1 M NaOH +0.05 M EDTA. This optimized analytical method using P NMR effectively identified phosphorus species in highly mineralized natural waters and can be applied to other highly mineralized lake waters globally.
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关键词
(31)P NMR,H resin,Mineralized water,Phosphorus speciation,Pretreatment method
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