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使用气相分子吸收光谱法对铵和硝酸盐进行顺序流动注射分析。

Sequential flow injection analysis of ammonium and nitrate using gas phase molecular absorption spectrometry.

作者信息

Haghighi B, Kurd S Farrokhi

机构信息

Department of Chemistry, Institute for Advanced Studies in Basic Sciences, P.O. Box 45195-159, Gava Zang, Zanjan, Iran.

出版信息

Talanta. 2004 Oct 20;64(3):688-94. doi: 10.1016/j.talanta.2004.03.037.

Abstract

A flow injection method on the basis of gas phase molecular absorption is described for the sequential determination of ammonium and nitrate. Two hundred microliters of sample solution is injected into the flow line. For ammonium determination, the sample zone is directed to a line in which reacts with NaOH (13M) and produces ammonia. But for nitrate determination, the sample zone is passed through the on-line copperized zinc (Zn/Cu) reduction column and produces ammonium ion and in the follows ammonia. The produced ammonia in both cases is purged into the stream of N(2) carrier gas. The gaseous phase is separated from the liquid phase using a gas-liquid separator and then is swept into a flow through cell, which has been positioned in the cell compartment of an UV-Vis spectrophotometer. The absorbance of the gaseous phase is measured at 194nm. Under selected conditions for sequential analysis of ammonium and nitrate, linear relations were found between the peak heights of absorption signals and concentrations of ammonium (10-650mugml(-1)) and nitrate (20-800mugml(-1)). The limit of detections for ammonium and nitrate analysis were 8 and 10mugml(-1), respectively. The relative standard deviations of repeated measurements of 50mugml(-1) of ammonium and nitrate were 2.0, 2.9%, respectively. Maximum sampling rate was about 40 samples/h. The method was applied to the determination of ammonium in pharmaceutical products and the sequential determination of ammonium and nitrate in spiked water samples.

摘要

描述了一种基于气相分子吸收的流动注射法,用于铵和硝酸盐的顺序测定。将200微升样品溶液注入流动管路。对于铵的测定,将样品区导入与氢氧化钠(13M)反应并产生氨的管路。但对于硝酸盐的测定,样品区通过在线镀铜锌(Zn/Cu)还原柱,产生铵离子,随后产生氨。两种情况下产生的氨被吹扫到氮气载气流中。使用气液分离器将气相与液相分离,然后吹扫到流通池中,该流通池已放置在紫外可见分光光度计的样品池中。在194nm处测量气相的吸光度。在选定的铵和硝酸盐顺序分析条件下,发现吸收信号的峰高与铵(10 - 650μg/ml(-1))和硝酸盐(20 - 800μg/ml(-1))浓度之间存在线性关系。铵和硝酸盐分析的检测限分别为8和10μg/ml(-1)。对50μg/ml(-1)的铵和硝酸盐进行重复测量的相对标准偏差分别为2.0%、2.9%。最大采样率约为40个样品/小时。该方法应用于药品中铵的测定以及加标水样中铵和硝酸盐的顺序测定。

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