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气相法测定用重氮甲烷预处理的2-甲基-3-硝基苯甲酸
引用本文:薛科社,南志祥.气相法测定用重氮甲烷预处理的2-甲基-3-硝基苯甲酸[J].色谱,2002,20(5):456-458.
作者姓名:薛科社  南志祥
作者单位:1. 西北大学环境科学系中心实验室,陕西,西安,710069
2. 西北大学化学系有机化学教研室,陕西,西安,710069
摘    要: 建立了一种采用气相测定 2 甲基 3 硝基苯甲酸含量的分析方法。用重氮甲烷对 2 甲基 3 硝基苯甲酸进行酯化预处理 ,以CP Sil 43CB石英毛细管柱 (2 5m× 0 32mmi d × 0 2 μm)分离 ,氢火焰离子化检测器检测 ,归一化法定量。平均回收率为 99 81 % ,相对标准偏差 (RSD)为 0 0 8% ,最低检出限为 3× 1 0 - 1 1 g。方法简便实用 ,稳定可靠 ,实现了用气相法对这种高沸点、高纯度物质的定量分析 ,可用于该类物质的纯度检验 ,也可用于新产品开发及生产、科研中的过程分析。

关 键 词:气相  2-甲基-3-硝基苯甲酸  重氮甲烷  酯化
文章编号:1000-8713(2002)05-0456-03
修稿时间:2001年10月30

Determination of 2-Methyl-3-Nitrobenzoic Acid Through Pretreatment with Diazomethane by Gas Chromatography
XUE Ke she ,NAN Zhi xiang.Determination of 2-Methyl-3-Nitrobenzoic Acid Through Pretreatment with Diazomethane by Gas Chromatography[J].Chinese Journal of Chromatography,2002,20(5):456-458.
Authors:XUE Ke she  NAN Zhi xiang
Institution:Experiment Center of Department of Environmental Science, Northwest University, Xi'an 710069, China. dlxgis@nwu.edu.cn
Abstract:A method for the quantitative determination of 2-methyl-3-nitrobenzoic acid by gas chromatography is described. 2-Methyl-3-nitrobenzoic acid was esterified by pretreatment with diazomethane prior to analysis. A CP-Sil-43CB capillary column(25 m x 0.32 mm i.d. x 0.2 microm), a flame ionization detector and the area normalization method were used. The average recovery was 99.81%. The RSD was 0.08% and the detection limit was 3 x 10(-11) g. The results showed that the method is practical and reliable. It was realized that the higher purity and higher boiler matter was analyzed by gas chromatography. The method can be used to monitor the purity of this type of materials. analysis of research and production. It can be used in the development of new products and in the process.
Keywords:gas chromatography  2  methyl  3  nitrobenzoic acid  diazomethane  esterification
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