气相色谱法测定用重氮甲烷预处理的2-甲基-3-硝基苯甲酸

Determination of 2-Methyl-3-Nitrobenzoic Acid Through Pretreatment with Diazomethane by Gas Chromatography

建立了一种采用气相色谱测定 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 ,实现了用气相色谱法对这种高沸点、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。

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×0 32 mm i d ×0 2 μm), 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 3×10 -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. It can be used in the development of new products and in the process analysis of research and production.