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灵敏分光光度法测定人唾液和雨水中的亚硝酸盐以及大气中的二氧化氮。

Sensitive spectrophotometric determination of nitrite in human saliva and rain water and of nitrogen dioxide in the atmosphere.

作者信息

Helaleh M I, Korenaga T

机构信息

University of Tokushima, Faculty of Integrated Arts and Sciences, Minami-Josanjima, Japan.

出版信息

J AOAC Int. 2001 Jan-Feb;84(1):53-8.

Abstract

A new simple, sensitive, and selective spectrophotometric method was developed for the determination of nitrite. The method is based on the reaction of nitrite with sulfathiazole in acidic medium to form a diazonium cation, which is subsequently coupled with N-(1-naphthyl)ethylenediamine dihydrochloride to form a highly stable, violet azo dye. The reaction product has an absorption maximum at 546 nm and obeys Beer's law over a nitrite range of 0.054-0.816 microg/mL. The molar absorptivity of the colored compound is 4.61 x 10(4) L/mol x cm). The detection limit is 12.1 microg/L. The relative standard deviation is 0.85% for 5 determinations of nitrite at 0.27 microg/mL. The reproducibility and validity of the proposed method are discussed in the present paper. The simplicity of the method is demonstrated by the high stability of the azo-dye product as well as the short time required for its complete formation in a reaction at room temperature without pH control or extra extraction. The sensitivity of the method is shown by the successful determination of nitrite in human saliva and rain water, and of nitrogen dioxide in the atmosphere. The results compare favorably with those obtained by the reference method. The selectivity of the method is indicated by its freedom from most interferences, even at high concentrations of nitrate (500 microg/mL).

摘要

开发了一种新的简单、灵敏且选择性好的分光光度法用于测定亚硝酸盐。该方法基于亚硝酸盐在酸性介质中与磺胺噻唑反应形成重氮阳离子,随后该重氮阳离子与盐酸N-(1-萘基)乙二胺偶合形成一种高度稳定的紫色偶氮染料。反应产物在546nm处有最大吸收,在0.054 - 0.816μg/mL的亚硝酸盐范围内符合比尔定律。有色化合物的摩尔吸光系数为4.61×10⁴L/mol·cm。检测限为12.1μg/L。对0.27μg/mL的亚硝酸盐进行5次测定时,相对标准偏差为0.85%。本文讨论了该方法的重现性和有效性。该方法的简便性体现在偶氮染料产物的高稳定性以及在室温下无需控制pH或额外萃取即可在短时间内完全形成反应。该方法的灵敏度体现在成功测定了人唾液和雨水中的亚硝酸盐以及大气中的二氧化氮。结果与参考方法获得的结果相比具有优势。该方法的选择性体现在即使在高浓度硝酸盐(500μg/mL)存在下也不受大多数干扰。

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