首页> 外国专利> METHOD OF HIGH-EFFICIENT LIQUID CHROMATOGRAPHIC DETERMINATION OF CONCENTRATIONS OF ALKYLPHOSPHONIC AND/OR O-ALKYLALKYLPHOSPHONIC ACIDS IN AQUEOUS SOLUTION

METHOD OF HIGH-EFFICIENT LIQUID CHROMATOGRAPHIC DETERMINATION OF CONCENTRATIONS OF ALKYLPHOSPHONIC AND/OR O-ALKYLALKYLPHOSPHONIC ACIDS IN AQUEOUS SOLUTION

机译:高效液相色谱法测定水溶液中烷基膦酸和/或邻烷基烷基膦酸的浓度

摘要

FIELD: chemistry.;SUBSTANCE: invention relates to the field of analytical chemistry, namely the quantification of low concentrations of O-alkylalkylphosphonic and/or alkylphosphonic acid in environmental objects and biological objects in order to establish the use of organophosphorus warfare agents. Claimed method comprises liquid chromatographic separation of said acids in a chromatographic column filled with a porous graphitized carbon sorbent, wherein the chromatographic column is used with a length of 30–150 mm. Chromatographic column is previously washed with water at a flow rate of 0.1–0.2 ml/min for at least 15 minutes, after that, the test aqueous solution is introduced into the sample column in an amount of 5–20 mcl at a flow rate of 0.1–0.2 ml/min. Then, an aqueous solution of formic acid with a concentration of 0.01–0.5 vol% is introduced at a flow rate of 0.1–0.2 ml/min for the elution of the sample introduced into the column, followed by the determination of the concentration of alkylphosphonic and/or O-alkylalkylphosphonic acids by a mass spectrometric method according to the calibration curve, previously constructed for alkylphosphonic and/or O-alkylalkylphosphonic acids in an aqueous solution.;EFFECT: increase in the coefficient of capacity (mass distribution coefficient), which leads to an increase in the resolution of analyte peaks on the chromatogram and to a higher accuracy and sensitivity of determining the concentration of acids.;8 cl, 5 dwg, 6 tbl
机译:发明领域本发明涉及分析化学领域,即定量确定环境物体和生物物体中低浓度的O-烷基烷基膦酸和/或烷基膦酸以确立有机磷战剂的用途。要求保护的方法包括在填充有多孔石墨化碳吸附剂的色谱柱中对所述酸进行液相色谱分离,其中色谱柱的长度为30-150 mm。色谱柱事先用水以0.1–0.2 ml / min的速度洗涤至少15分钟,之后,将测试水溶液以5–20 mcl的量引入到样品柱中,流速为0.1–0.2毫升/分钟。然后,以0.1–0.2 ml / min的流速引入浓度为0.01–0.5 vol%的甲酸水溶液,以洗脱引入色谱柱中的样品,然后确定烷基膦酸的浓度和/或O-烷基烷基膦酸根据校准曲线通过质谱方法制备,以前是针对水溶液中的烷基膦酸和/或O-烷基烷基膦酸构建的;效果:增加容量系数(质量分布系数),导致色谱图上分析物峰的分辨率提高,并提高了测定酸浓度的准确性和灵敏度.8 cl,5 dwg,6 tbl

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