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采用离子对高效液相色谱法测定天然水中的膦酸盐。

Determination of phosphonates in natural waters by ion-pair high-performance liquid chromatography.

作者信息

Nowack B

机构信息

Swiss Federal Laboratories for Materials Testing and Research (EMPA), St. Gallen, Switzerland.

出版信息

J Chromatogr A. 1997 Jun 27;773(1-2):139-46. doi: 10.1016/s0021-9673(97)00202-1.

Abstract

The paper describes a new method for the determination of phosphonates by ion-pair high-performance liquid chromatography. The phosphonates are complexed with Fe(III) and separated on a reversed-phase polymer column. The eluent consists of a bicarbonate solution at pH 8.3, tetrabutylammoniumbromide as counter-ion and 14% acetonitrile. The complexes are detected at 260 nm. The four phosphonates HEDP (1-hydroxyethylene-1,1-diphosphonic acid). ATMP (aminotris [methylenephosphonic acid]), EDTMP [ethylenediaminetetra(methylenephosphonic acid)], and DTPMP [diethylenetriaminepenta (methylenephosphonic acid)] are well separated within 20 min. The limits of detection are 5.10(-8) M for ATMP and EDTMP, 1.10(-7) M for DTPMP and 5.10(-7) M for HEDP. The method is suitable for the determination of phosphonates in the influent and effluent of wastewater treatment plants. A preconcentration of 10 is easily achieved by adsorption of the phosphonates onto freshly precipitated calcium carbonate and subsequent dissolution of the solid-phase by HCl.

摘要

本文描述了一种通过离子对高效液相色谱法测定膦酸盐的新方法。膦酸盐与Fe(III)络合,并在反相聚合物柱上分离。洗脱液由pH 8.3的碳酸氢盐溶液、作为抗衡离子的四丁基溴化铵和14%的乙腈组成。络合物在260 nm处检测。四种膦酸盐HEDP(1-羟基乙叉-1,1-二膦酸)、ATMP(氨基三亚甲基膦酸)、EDTMP [乙二胺四(亚甲基膦酸)]和DTPMP [二乙烯三胺五(亚甲基膦酸)]在20分钟内得到很好的分离。ATMP和EDTMP的检测限为5×10⁻⁸ M,DTPMP为1×10⁻⁷ M,HEDP为5×10⁻⁷ M。该方法适用于测定污水处理厂进水和出水中的膦酸盐。通过将膦酸盐吸附到新沉淀的碳酸钙上,随后用HCl溶解固相,很容易实现10倍的预浓缩。

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