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针式萃取结合气相色谱-屏障放电电离检测吹扫捕集法测定水样中的氨

Purge-and-trap Determination of Ammonia in Water Samples Using Needle-type Extraction Coupled with Gas Chromatography-Barrier Discharge Ionization Detection.

作者信息

Ueta Ikuo, Fujikawa Hiroto, Fujimura Koji, Saito Yoshihiro

机构信息

Department of Applied Chemistry, University of Yamanashi.

Shinwa Chemical Industries Ltd.

出版信息

Anal Sci. 2019 Jul 10;35(7):759-762. doi: 10.2116/analsci.19P016. Epub 2019 Mar 22.

Abstract

This manuscript describes the determination of ammonia (NH) in aqueous samples by purge-and-trap extraction using a needle-type extraction device with gas chromatography-barrier discharge ionization detector (GC-BID). NH was purged from the aqueous samples in basic conditions and then salted out with sodium chloride. Purged ammonia was trapped onto non-volatile carboxylic acid-coated macroporous terephthalic acid particles, which were contained within the needle-type extraction device. The analyte (NH) was thermally desorbed by heating the extraction needle in the GC injection port, and detected by BID. After the optimization of both purge and extraction conditions, the linearity and sensitivity of the proposed method were evaluated. The limit of detection was found to be 2.0 mg L at a headspace sampling volume of 100 mL. The method applicability was confirmed by the determination of spiked NH in tap water and river water samples.

摘要

本手稿描述了使用带有气相色谱-屏障放电电离检测器(GC-BID)的针型萃取装置,通过吹扫捕集萃取法测定水性样品中的氨(NH₃)。在碱性条件下从水性样品中吹扫出NH₃,然后用氯化钠进行盐析。吹扫出的氨被捕集到针型萃取装置内的非挥发性羧酸涂层大孔对苯二甲酸颗粒上。通过在GC进样口中加热萃取针使分析物(NH₃)热脱附,并由BID进行检测。在优化吹扫和萃取条件后,对所提出方法的线性和灵敏度进行了评估。在顶空进样体积为100 mL时,检测限为2.0 mg/L。通过测定自来水和河水样品中加标的NH₃,证实了该方法的适用性。

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